A method for recovering by-product ammonium chloride in a production process of kresoxim-methyl

Abstract

The application relates to the field of pesticide environmental protection technology, and discloses a recovery method for byproduct ammonium chloride in the production process of kresoxim-methyl, which comprises a device main body, a distillation unit is fixedly arranged at the top end of the device main body, a water isolation unit is fixedly arranged at the bottom end of the distillation unit, a flow guide unit is fixedly arranged at the bottom end of the water isolation unit, a heating unit is fixedly arranged outside the flow guide unit, a heat dissipation unit is fixedly arranged at the bottom end of the heating unit, a filter unit is fixedly arranged inside the heat dissipation unit, a vibration unit is fixedly arranged in the filter unit, and a liquid storage bin is fixedly arranged at the bottom end of the filter unit. Through the working of the water isolation unit, small water droplets are wiped through the water isolation unit after being condensed at the bottom end steam inlet of the distiller in the distillation process, the backflow of the liquefied water droplets is prevented, the concentration of the bottom end liquid medicine is influenced, the liquid medicine can be treated at an accurate concentration, and the problem that the treatment result of the subsequent step is greatly deviated is avoided.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of pesticide environmental protection technology, in particular to a method for recovering by-product ammonium chloride in the production process of kresoxim-methyl. BACKGROUND

[0002] A fungicide has broad-spectrum fungicidal activity, good protection and treatment, no cross resistance with other commonly used fungicides, longer persistence than conventional fungicides, high selectivity, safety to crops, humans and animals, and no environmental pollution.

[0003] The existing method for recovering by-product ammonium chloride in the production process of kresoxim-methyl has the following problems in the implementation process of a certain technology:

[0004] 1. 50g of kresoxim-methyl by-product ammonium chloride crude product (containing 40g of ammonium chloride), 100g of water and 25g of toluene are added to a 500ml four-necked bottle, stirred to 70℃ and reacted for 1h, then static for 30min, layered, collected the organic phase, and the organic phase was distilled to 95℃, and the solvent was distilled to recover 0.64g of intermediate 2-(2-methylphenoxy methyl) phenyl oxalate methyl ester (content 78%), and the recovered solvent can be continuously used. During the distillation process, the temperature and pressure in the container will increase. When the temperature rises, the water vapor is separated through the distillation device. However, during the separation process, there are residual water droplets at the inlet of the distillation device. Generally, a conventional distillation device is used for distillation or the container is opened for wiping. However, these methods cannot avoid the attachment of water droplets on the inner wall after distillation, and even the reflux into the liquid, which affects the purity of the liquid and even the preparation of the subsequent process, resulting in problems in the preparation results and difficulty in ensuring the quality.

[0005] 2. After the water phase is filtered at 60℃, the filtrate is cooled to 2℃, and high-purity ammonium chloride 16.6g is obtained by centrifugation. During the filtration process, the filtration effect of the filter screen is gradually reduced after long-term repeated filtration. Generally, the filter screen is replaced or cleaned. However, these methods need to be operated manually to clean completely, which consumes a lot of time and money, and wastes manpower and maintenance cost. SUMMARY

[0006] The present application relates to the field of pesticide environmental protection technology, in particular to a method for recovering by-product ammonium chloride in the production process of kresoxim-methyl.

[0007] In order to achieve the above object, the present application provides the following technical scheme: a kind of kresoxim-methyl production process by-product ammonium chloride recovery method, including device main body, the top of the device main body is fixedly provided with distillation unit, the bottom of the distillation unit is fixedly provided with water isolation unit, the bottom of the water isolation unit is fixedly provided with flow guide unit, the outside of the flow guide unit is fixedly provided with heating unit, the bottom of the heat unit is fixedly provided with filter unit, the inside of the filter unit is fixedly provided with vibration unit, the bottom of the filter unit is fixedly provided with liquid storage bin.

[0008] Preferably, the water isolation unit includes a water pan, the inner side of the outer wall of the water pan is fixedly provided with six water guide rods, the inner side of the inner wall of the water pan is fixedly connected with an auxiliary slide, the inside of the auxiliary slide is slidably connected with a sliding block, the side of the sliding block is fixedly connected with a connecting soft belt, the top end of the connecting soft belt is slidably connected with a reverse bevel gear, the top end of the reverse bevel gear is engagedly connected with a rotating gear, the side of the rotating gear is fixedly connected with a wiping plate, and the bottom end of the connecting soft belt is fixedly connected to the inner side of the inner wall of the water pan.

[0009] Preferably, the flow guide unit includes a side-tilting flow guide plate, the outer side of the side-tilting flow guide plate is fixedly provided with a flow guide housing, the top surface of the side-tilting flow guide plate is fixedly provided with a flow guide vertical plate, the top end of the flow guide vertical plate is slidably connected with a buoyancy block, the side end of the buoyancy block is fixedly provided with a sliding disc, the sliding disc is slidably connected inside two flow guide slides, the flow guide slides are fixedly connected to the inner wall of the flow guide housing, the side end bottom surface of the side-tilting flow guide plate is fixedly connected with a flow guide spring, and the bottom end of the flow guide spring is fixedly connected with a flow guide bottom plate.

[0010] Preferably, the filter unit includes a filter housing, the inside of the bottom end of the filter housing is fixedly provided with a filter screen, the side end of the filter screen is rotatably connected with a pressing plate, the bottom end of the pressing plate is fixedly connected with a filter residue collection box, the top end side of the filter screen is slidably connected with a cleaning telescopic plate, the top end of the cleaning telescopic plate is fixedly connected with a translation motor, the side of the cleaning telescopic plate is fixedly connected with a filter residue sensor, the inside of the translation motor is threadedly connected with a translation screw rod, the side of the pressing plate is rotatably connected with a pressing plate rotating shaft, the bottom end of the pressing plate rotating shaft and the pressing plate are fixedly connected with a return spring, and the side end of the pressing plate is fixedly connected with a pressing block.

[0011] Preferably, the vibration unit includes a vibration motor, the top and bottom ends of the vibration motor are fixedly connected with fixed plates, the side ends of the two fixed plates are fixedly connected with vibration slides, the inside of the top vibration slide is slidably connected with a top slide rod, the bottom end of the top slide rod is rotatably connected with a top auxiliary rod, the bottom end of the top auxiliary rod is rotatably connected to a vibration disc, the inside of the bottom vibration slide is slidably connected with a bottom slide rod, the top end of the bottom slide rod is rotatably connected with a bottom rotating rod, the top end of the bottom rotating rod is rotatably connected to the vibration disc, and the side end of the vibration disc is fixedly connected to the output end of the vibration motor.

[0012] (I) Advantages

[0013] Compared with the prior art, the present application provides a method for recovering the by-product ammonium chloride in the production process of kresoxim-methyl, which has the following advantages:

[0014] 1. The method for recovering the by-product ammonium chloride in the production process of kresoxim-methyl can clean the small water droplets condensed at the bottom end of the distiller during the distillation process through the wiping of the water separation unit, and the small water droplets can be collected and stored through the water pan, preventing the backflow of liquefied water droplets from affecting the concentration of the liquid at the bottom end, so that the liquid can be treated at the accurate concentration, ensuring that the subsequent processing results are more accurate and accurate.

[0015] 2. The method for recovering the by-product ammonium chloride in the production process of kresoxim-methyl can clean the filter residue accumulated on the top of the filter screen during the filtering step, avoiding the influence of the filter residue on the operation of the overall device, and timely cleaning of the filter residue can also ensure the working efficiency of the filter screen, prolong the service life of the filter screen, and avoid the consumption of a large amount of time and funds when replacing and cleaning the filter screen.

[0016] 3. The method for recovering the by-product ammonium chloride in the production process of kresoxim-methyl, through the working of the vibration unit, in the special case that the filter screen has been used for a long time and a large amount of residue appears in the filter screen mesh, the vibration unit is used to shake and clean the residue inside the filter screen, which restores the normal filtering effect of the filter screen, prolongs the service life of the filter screen, and avoids replacing or cleaning the filter screen, wasting time and financial resources. BRIEF DESCRIPTION OF DRAWINGS

[0017] The present application will be further described below in conjunction with the drawings and examples.

[0018] Figure 1 is a front side perspective view.

[0019] Figure 2 is a perspective view of the inside of the filter unit.

[0020] Figure 3 is a perspective view of the inside of the water separation unit.

[0021] Figure 4 is Figure 3 is a local enlarged view of position A in FIG.

[0022] Figure 5 is a perspective view of the inside of the flow guide unit.

[0023] Figure 6 is a perspective view of the filter unit.

[0024] Figure 7 isFigure 6 Local enlarged view at B.

[0025] Figure 8 Perspective view of the vibration unit.

[0026] Figure 9 Perspective view of the flow guide unit. Figure 8 Local enlarged view at C.

[0027] Figure 10 Perspective view of the flow guide unit.

[0028] In the figure: 1, device main body; 2, distillation unit; 3, water separation unit; 301, water storage tray; 302, water guide rod; 303, auxiliary slide; 304, sliding block; 305, connecting soft belt; 306, reverse bevel gear; 307, rotating gear; 308, wiping plate; 4, flow guide unit; 401, lateral tilting flow guide plate; 402, flow guide shell; 403, flow guide vertical plate; 404, buoyancy block; 405, sliding disc; 406, flow guide slide; 407, flow guide spring; 408, flow guide bottom plate; 5, heating unit; 6, filtering unit; 601, filtering shell; 602, filter screen; 603, lower pressing plate; 604, filter residue collection box; 605, cleaning telescopic plate; 606, horizontal movement motor; 607, filter residue inductor; 608, horizontal movement screw; 609, pressing plate rotating shaft; 610, return spring; 611, lower pressing block; 7, vibration unit; 701, vibration motor; 702, fixed plate; 703, vibration slide; 704, top slide rod; 705, top auxiliary rod; 706, vibration disc; 707, bottom slide rod; 708, bottom rotating rod; 8, liquid storage bin. DETAILED DESCRIPTION

[0029] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0030] Please refer to Figure 1 A method for recovering by-product ammonium chloride in the production process of kresoxim-methyl, comprising a device main body 1, the top of the device main body 1 is fixedly provided with a distillation unit 2, the bottom of the distillation unit 2 is fixedly provided with a water separation unit 3, the bottom of the water separation unit 3 is fixedly provided with a flow guide unit 4, the outer side of the flow guide unit 4 is fixedly provided with a heating unit 5, the bottom of the heating unit 5 is fixedly provided with a filtering unit 6, the inside of the filtering unit 6 is fixedly provided with a vibration unit 7, and the bottom of the filtering unit 6 is fixedly provided with a liquid storage bin 8.

[0031] Please refer toFigure 2 , Figure 3 ,and Figure 4 The water-blocking unit 3 includes a water storage tray 301. Six water guide rods 302 are fixedly installed on the inner side of the outer wall of the water storage tray 301. An auxiliary slide 303 is fixedly connected to the inner side of the inner wall of the water storage tray 301. A sliding block 304 is slidably connected inside the auxiliary slide 303. A connecting soft band 305 is fixedly connected to the side of the sliding block 304. A reverse bevel tooth 306 is slidably connected to the top of the connecting soft band 305. A rotating gear 307 is meshed with the top of the reverse bevel tooth 306. A wiping plate 308 is fixedly connected to the side of the rotating gear 307. The bottom end of the connecting soft band 305 is fixedly connected to the inner side of the inner wall of the water storage tray 301.

[0032] Please see Figure 5 and Figure 10 The flow guiding unit 4 includes a side-tilting flow guiding plate 401. A flow guiding shell 402 is fixedly installed on the outer side of the side-tilting flow guiding plate 401. A flow guiding upright plate 403 is fixedly installed on the top surface of the side-tilting flow guiding plate 401. A buoyancy block 404 is slidably connected to the top of the flow guiding upright plate 403. A sliding disc 405 is fixedly installed on the side end of the buoyancy block 404. The sliding disc 405 is slidably connected inside two flow guiding channels 406. The flow guiding channels 406 are fixedly connected to the inner wall of the flow guiding shell 402. A flow guiding spring 407 is fixedly connected to the bottom surface of the side end of the side-tilting flow guiding plate 401. A flow guiding base plate 408 is fixedly connected to the bottom end of the flow guiding spring 407.

[0033] Please see Figure 6 , Figure 8 and Figure 9 The filter unit 6 includes a filter housing 601, a filter screen 602 fixedly disposed inside the bottom end of the filter housing 601, a lower pressure plate 603 rotatably connected to the side end of the filter screen 602, a filter residue collection box 604 fixedly connected to the bottom end of the lower pressure plate 603, a cleaning telescopic plate 605 slidably connected to the side of the top end of the filter screen 602, a translational motor 606 fixedly connected to the top end of the cleaning telescopic plate 605, a filter residue sensor 607 fixedly connected to the side of the cleaning telescopic plate 605, a translational screw 608 threadedly connected inside the translational motor 606, a pressure plate shaft 609 rotatably connected to the side of the lower pressure plate 603, a return spring 610 fixedly connected to the pressure plate shaft 609 and the bottom end of the lower pressure plate 603, and a lower pressure block 611 fixedly connected to the side end of the lower pressure plate 603.

[0034] Please see Figure 6 and Figure 7The vibration unit 7 comprises a vibration motor 701, both upper and lower ends of the vibration motor 701 are fixedly connected with fixed plates 702, both sides of the two fixed plates 702 are fixedly connected with vibration slides 703, the inside of the top vibration slide 703 is slidably connected with a top slide rod 704, the bottom end of the top slide rod 704 is rotatably connected with a top auxiliary rod 705, the bottom end of the top auxiliary rod 705 is rotatably connected with a vibration disc 706, the inside of the bottom vibration slide 703 is slidably connected with a bottom slide rod 707, the top end of the bottom slide rod 707 is rotatably connected with a bottom rotating rod 708, the top end of the bottom rotating rod 708 is rotatably connected with the vibration disc 706, and the side end of the vibration disc 706 is fixedly connected with the output end of the vibration motor 701.

[0035] When the raw material is treated, the raw material is first poured into the device main body 1, heated and distilled by the heating unit 5, distilled by the distillation unit 2 during the distillation process, and the small water droplets are formed on the inner wall of the bottom end of the distillation unit 2 after the distillation is completed, at this time, the small water droplets gradually increase, the water droplets are guided into the water pan 301 by the water guide rod 302, and the water in the water pan 301 is collected.

[0036] In the present application, when the distillation process is about to end, the raw material after distillation and dehydration is guided into the bottom filtering unit 6 for filtering by the flow guide unit 4 at this time, because the water gradually decreases during the distillation process, the liquid level of the top of the flow guide unit 4 gradually decreases, thereby driving the buoy block 404 to descend, the buoy block 404 descends and fluctuates the flow guide vertical plate 403, thereby enabling the buoy block 404 to move downward under the cooperation of the sliding disc 405 and the flow guide slide 406, thereby enabling the side-tilting flow guide plate 401 to be inclined, and the liquid is poured into the inside of the bottom filtering unit 6, and after the liquid is poured, the flow guide spring 407 is reset.

[0037] When the filtering unit 6 is ready to filter in the application, the filter screen 602 filters the filter residue, and the filtrate flows into the lower liquid storage bin 8, at this time, a large amount of filter residue remains on the top of the filter screen 602, when the top surface of the filter residue touches the filter residue sensor 607, the horizontal motor 606 starts to move, and moves through the horizontal screw rod 608, and then drives the bottom cleaning telescopic plate 605 to move, the cleaning telescopic plate 605 telescopes according to the width of the filter screen 602 during the horizontal movement, and all the filter residue is cleaned to the top surface of the lower pressing plate 603, when a certain amount of filter residue is accumulated on the top surface of the lower pressing plate 603, the lower pressing plate 603 is pressed down through the auxiliary of the lower pressing block 611, the filter residue is collected and recycled by the inclined lower pressing plate 603, and the filtering process steps are completed.

[0038] In the application, after a long time of using the same filtering unit, a large amount of residue will accumulate in the filter screen 602, and the filtering unit 6 is difficult to clean in this special case, at this time, the vibration unit 7 is used for cleaning, the vibration motor drives the vibration disc 706 to rotate after starting, the top auxiliary rod 705 and the bottom rotating rod 708 on the side of the vibration disc 706 move, and then the top sliding rod 704 and the bottom sliding rod 707 move up and down at the same time, and then the side tilt guide plate 401 and the filter screen 602 vibrate up and down at the same time, so that not only the residue in the filter screen 602 can be cleaned, but also the liquid medicine easily remaining on the top of the side tilt guide plate 401 can be vibrated and cleaned, which is convenient and fast.

[0039] In the description of the application, unless otherwise explicitly specified and limited, the "arrangement", "installation", "connection", "connection", "fixing" should be understood in a broad sense, for example, it can be fixed connection, or detachable connection, or integrated; it can be mechanical connection, or electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or the internal communication of two elements or the interaction relationship between two elements. For ordinary skilled in the art, the above belonging to the specific meaning in the application can be understood according to the specific circumstances.

[0040] The standard parts used in the application can be purchased from the market, and the special-shaped parts can be customized according to the description and the drawings.

[0041] The above is only the preferred specific embodiment of the application, but the protection scope of the application is not limited to this, any skilled in the art can make equivalent replacement or change according to the technical scheme and the inventive concept of the application within the technical range disclosed by the application, which should be covered in the protection scope of the application.

Claims

1. A recovery device for the by-product ammonium chloride in the production process of kresoxim-methyl, comprising a device main body (1), characterized in that: The device body (1) top fixedly provided with distillation unit (2), the distillation unit (2) bottom fixedly provided with water isolation unit (3), the water isolation unit (3) bottom fixedly provided with flow guide unit (4), the flow guide unit (4) outside fixedly provided with heating unit (5), the heating unit bottom fixedly provided with filter unit (6), the filter unit (6) inside fixedly provided with vibration unit (7), the filter unit (6) bottom fixedly provided with liquid storage bin (8);The water isolation unit (3) includes a water pan (301), the water pan (301) outer wall inside fixedly provided with six water guide bars (302), the water pan (301) inner wall inside fixedly connected with auxiliary slide (303), the auxiliary slide (303) inside slidingly connected with sliding block (304), the sliding block (304) side fixedly connected with connecting soft belt (305), the connecting soft belt (305) top slidingly connected with reverse bevel gear (306), the reverse bevel gear (306) top meshing connection has rotating gear (307), the rotating gear (307) side fixedly connected with wiping plate (308), the connecting soft belt (305) bottom fixedly connected in the water pan (301) inner wall inside;The filter unit (6) includes a filter housing (601), the filter housing (601) bottom inside fixedly provided with filter screen (602), the filter screen (602) side end rotationally connected with lower pressing plate (603), the lower pressing plate (603) bottom fixedly connected with filter residue collection box (604), the filter screen (602) top side slidingly connected with cleaning telescopic plate (605), the cleaning telescopic plate (605) top fixedly connected with translation motor (606), the cleaning telescopic plate (605) side fixedly connected with filter residue sensor (607), the translation motor (606) inside screwedly connected with translation screw (608), the lower pressing plate (603) side rotationally connected with pressing plate pivot (609), the pressing plate pivot (609) and lower pressing plate (603) bottom fixedly connected with return spring (610), the lower pressing plate (603) side end fixedly connected with lower pressing block (611).The vibration unit (7) includes a vibration motor (701), both upper and lower ends of the vibration motor (701) are fixedly connected with fixed plates (702), both sides of the two fixed plates (702) are fixedly connected with vibration slides (703), the inside of the top vibration slide (703) is slidably connected with a top slide rod (704), the bottom end of the top slide rod (704) is rotatably connected with a top auxiliary rod (705), the bottom end of the top auxiliary rod (705) is rotatably connected on a vibration disc (706), the inside of the bottom vibration slide (703) is slidably connected with a bottom slide rod (707), the top end of the bottom slide rod (707) is rotatably connected with a bottom rotating rod (708), the top end of the bottom rotating rod (708) is rotatably connected on the vibration disc (706), and the side end of the vibration disc (706) is fixedly connected on the output end of the vibration motor (701).

2. The device for recovering the by-product ammonium chloride in the process of producing kresoxim-methyl according to claim 1, characterized in that: The flow guide unit (4) comprises a side-tilting flow guide plate (401), a flow guide outer shell (402) is fixedly arranged outside the side-tilting flow guide plate (401), a flow guide vertical plate (403) is fixedly arranged on the top surface of the side-tilting flow guide plate (401), a buoyancy block (404) is slidably connected to the top end of the flow guide vertical plate (403), a sliding disc (405) is fixedly arranged on the side end of the buoyancy block (404), the sliding disc (405) is slidably connected inside two flow guide slides (406), the flow guide slides (406) are fixedly connected to the inner wall of the flow guide outer shell (402), a flow guide spring (407) is fixedly connected to the bottom surface of the side end of the side-tilting flow guide plate (401), and a flow guide bottom plate (408) is fixedly connected to the bottom end of the flow guide spring (407).

3. The use of a device for recovering by-product ammonium chloride in the process of producing kresoxim-methyl according to claim 2, characterized in that: The specific steps of the recovery method for the by-product ammonium chloride in the production process of kresoxim-methyl are as follows: S1: When the raw material is processed, first pour the raw material into the device main body (1), heat and distill through the heating unit (5), distill through the distillation unit (2) during the distillation process, and after the distillation is completed, small water droplets are easily formed on the inner side wall at the bottom end of the distillation unit (2), at this time the small water droplets gradually increase, the water droplets are guided into the water pan (301) through the water guide rod (302), and after the water in the water pan (301) is collected, water droplets are still left on the inner wall, at this time, due to the increase of water droplets in the water pan (301), the water pan (301) gradually moves downward due to the action of gravity, thereby moving the sliding block (304) upward, thereby moving the connecting soft belt (305), thereby rotating the reverse bevel gear (306), thereby rotating the reverse bevel gear (306) to drive the rotating gear (307), and thereby wiping the inner wall with the wiping plate (308), and the excess water falls into the water pan (301); S2: When the distillation process is about to end, at this time, the raw material after dehydration is guided into the bottom-end filtering unit (6) for filtering through the flow guide unit (4), at this time, due to the gradual decrease of water quantity in the distillation process, the liquid level on the top of the flow guide unit (4) gradually decreases, thereby driving the buoyancy block (404) to descend, the buoyancy block (404) descends thereby fluctuating the flow guide vertical plate (403), thereby enabling the buoyancy block (404) to move downward under the cooperation of the sliding disc (405) and the flow guide slide (406), thereby causing the side-tilting flow guide plate (401) to tilt, and the liquid is poured into the inside of the bottom-end filtering unit (6), and after the liquid pouring is completed, the flow guide spring (407) is reset. S3: When the filter unit (6) is ready to filter, the filter screen (602) filters the filter residue, and the filtrate flows into the lower storage tank (8). At this time, a large amount of filter residue remains on the top of the filter screen (602), and when the top surface of the filter residue touches the filter residue sensor (607), the horizontal motor (606) starts to move, and the horizontal movement is realized through the horizontal screw rod (608), which in turn drives the bottom cleaning telescopic plate (605) to move. The cleaning telescopic plate (605) retracts during the horizontal movement according to the width of the filter screen (602), and all the filter residue is cleaned onto the top surface of the lower pressing plate (603). When the lower pressing plate (603) accumulates a certain amount of filter residue, the lower pressing plate (603) is pressed down with the assistance of the lower pressing block (611), and the filter residue is collected and recycled by the inclined lower pressing plate (603). The filtering process is completed. S4: After using the same filter unit (6) for a long time, a large amount of residue will accumulate inside the filter screen (602). In this special case, the filter unit (6) is difficult to clean, so the vibration unit (7) is used for cleaning. After the vibration motor is started, the vibration disc (706) rotates, and the top auxiliary rod (705) and the bottom rotating rod (708) on the side of the vibration disc (706) move, which in turn drives the top sliding rod (704) and the bottom sliding rod (707) to move up and down simultaneously and sequentially, and then the side-tilting guide plate (401) and the filter screen (602) are vibrated up and down. This not only cleans the residue in the filter screen (602), but also cleans the liquid medicine easily accumulated on the top of the side-tilting guide plate (401), which is convenient and fast.

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