An acetochlor production line and its production process

Abstract

The present application discloses an acetochlor production line and its production process, which relates to the field of pesticide production devices. The production line includes a raw material tank, an etherification reaction kettle, an acylation reaction kettle, a condensation reaction kettle, and a technical material tank that are sequentially connected through pipelines. An inspection device is provided between the condensation reaction kettle and the technical material tank; the inspection device includes a transparent container connected between the condensation reaction kettle and the technical material tank, an irradiation lamp and an imaging module for obtaining and comparing the imaging of the mixed liquid in the transparent container, and a control module for controlling the liquid inlet and outlet of the transparent container according to the imaging of the imaging module. The acetochlor production line of the present application can monitor the situation of the mixed liquid in the condensation reaction kettle during the entire stage when the intermediate chloromethyl ethyl ether, primary amide, and lye are mixed and undergo a condensation reaction in the condensation reaction kettle, and control the on-off of the liquid path between the condensation reaction kettle and the technical material tank according to the real-time monitoring results, effectively reducing production losses.

Description

Technical Field

[0001] This application relates to the field of pesticide production equipment, and particularly to an acetochlor production line and its production process. Background Art

[0002] Acetochlor is an amide - type selective, pre - emergence herbicide, which is an inhibitor of weed nucleic acid metabolism and protein synthesis. Its synthesis process mainly uses the methylene method.

[0003] Currently, the production process of acetochlor mainly includes the following steps: (1) Preparation of the intermediate chloromethyl ethyl ether: In a mixed solution of formaldehyde or paraformaldehyde and ethanol, HCL gas is introduced to obtain the intermediate chloromethyl ethyl ether; (2) Preparation of the intermediate 2 - ethyl - 6 - methyl - N - (2 - chloroacetyl) aniline (referred to as primary amide): 2 - ethyl - 6 - methyl aniline (MEA) reacts with an appropriate acylating agent to form the primary amide; (3) Synthesis of acetochlor: The intermediate chloromethyl ethyl ether and the primary amide undergo a condensation reaction in an alkaline solution to form the crude acetochlor. All of the above steps are operated in batch reaction kettles, and the reaction kettles are connected in series through pipelines according to the production process sequence to transfer each mixed solution during the preparation process.

[0004] In the actual production process, when the temperature of the mixed solution of the intermediate chloromethyl ethyl ether and the primary amide mixed solvent and the alkaline solution is higher than the normal reaction temperature (generally 30 - 40 °C) / the single - addition amount of the primary amide is relatively large / the addition rate of the intermediate chloromethyl ethyl ether is relatively slow, the condensation reaction of the intermediate chloromethyl ethyl ether and the primary amide in the alkaline solution is prone to side reactions, and white crystals insoluble in benzene - ring organic solvents appear in the benzene oil. The appearance of these white crystals not only affects the yield of the condensation reaction, greatly increases the consumption of raw materials, but also affects the internal quality of the crude acetochlor, resulting in the final product not meeting the quality indicators; in the current production process flow / the existing acetochlor production line, the inspection of the quality of the crude acetochlor product is generally located at the end of the production line, and the inspection is not timely enough, which is likely to cause production losses. Summary of the Invention

[0005] In order to improve the timeliness of the inspection of the white crystals that may be generated during acetochlor production, this application provides an acetochlor production line and its production process.

[0006] An acetochlor production line provided by this application adopts the following technical solutions:

[0007] An acetochlor production line includes a raw material tank, an etherification reactor, an acylation reactor, a condensation reactor, and a technical material tank that are connected in sequence through pipelines. The condensation reactor is used for the condensation reaction of intermediate chloromethyl ethyl ether, primary amide, and lye. The technical material tank is used for temporarily storing acetochlor technical material. An inspection device is provided between the condensation reactor and the technical material tank. The inspection device includes: a transparent container connected between the condensation reactor and the technical material tank; an irradiation lamp arranged above the transparent container; an imaging module arranged below the transparent container and used to cooperate with the irradiation lamp to obtain the optical imaging of the solution in the transparent container, and an image of a qualified mixed solution is preset in the imaging module; a control module arranged between the transparent container and the condensation reactor and between the transparent container and the technical material tank and used to control the liquid inlet and outlet of the transparent container according to the imaging of the imaging module.

[0008] By adopting the above technical solution, in the process of producing acetochlor, the raw material tank is used for raw material supply, intermediate chloromethyl ethyl ether is prepared in the etherification reactor, primary amide is prepared in the acylation reactor, and intermediate chloromethyl ethyl ether, primary amide, and lye are mixed in the condensation reactor to generate acetochlor technical material. During the whole stage of the mixing and condensation reaction of intermediate chloromethyl ethyl ether, primary amide, and lye in the condensation reactor, the control module is used to control the opening of the passage between the condensation reactor and the transparent container and the closing of the passage between the transparent container and the technical material tank, continuously introduce the mixed solution of intermediate chloromethyl ethyl ether, primary amide, and lye that is just mixed, in the process of mixing / reaction, and after mixing / reaction into the transparent container, and continuously irradiate the transparent container with the irradiation lamp, and at the same time use the imaging module to obtain the optical imaging of the transparent container and the mixture in the transparent container by the irradiation lamp. At the same time, the control module compares the imaging obtained by the imaging module with the standard image of the mixed solution without white crystals preset in the imaging module, intermittently images and detects the mixed solution of intermediate chloromethyl ethyl ether, primary amide, and lye during the whole process of the condensation reaction, timely judges and identifies whether white crystals are generated in the mixed solution, and controls the on-off of the liquid path between the condensation reactor and the technical material tank according to the real-time monitoring results, effectively reducing production losses.

[0009] Optionally, a liquid inlet pipe connecting the condensation reactor and the transparent container, a technical material discharge pipe connecting the transparent container and the technical material tank, and a waste liquid discharge pipe are provided on the transparent container. The waste liquid discharge pipe is connected to a waste liquid tank. The control module includes a first electromagnetic control valve, a second electromagnetic control valve, and a third electromagnetic control valve respectively arranged on the liquid inlet pipe, the technical material discharge pipe, and the waste liquid discharge pipe, and a PLC control system used to control the first electromagnetic control valve, the second electromagnetic control valve, and the third electromagnetic control valve. The PLC control system is electrically connected to the imaging module.

[0010] By adopting the above technical solution, during the real-time monitoring of whether there are white crystals in the transparent container by the irradiation lamp and the imaging module, the PLC control system can correspondingly control the first electromagnetic control valve, the second electromagnetic control valve, and the third electromagnetic control valve to open / close the liquid inlet pipe, the raw drug discharge pipe, and the waste liquid discharge pipe, so as to more conveniently realize the on / off of the liquid path between the condensation reactor and the transparent container, between the transparent container and the raw drug tank, and between the transparent container and the waste liquid tank, which is beneficial for the operator to adjust and control the temperature / single addition amount of primary amide / the addition speed of intermediate chloromethyl ethyl ether in the condensation reactor in real time according to the monitoring and comparison situation of the imaging module.

[0011] Optionally, the top wall and the bottom wall of the transparent container are both horizontally arranged, and a pressure filtration device is provided in the transparent container for pressure-filtering the white crystals in the waste liquid from top to bottom when there are white crystals in the transparent container.

[0012] By adopting the above technical solution, when there are white crystals in the transparent container, the pressure filtration device is used to pressure-filter the mixed liquid from top to bottom, which can separate the waste liquid and the white crystals, so as to remove the white crystals in the waste liquid and recycle the waste liquid obtained by pressure filtration without white crystals.

[0013] Optionally, the pressure filtration device includes a fixed frame, a transparent pressure filtration membrane arranged in the fixed frame, and a linear driving member for driving the fixed frame to lift. A plurality of micropores are formed through the transparent pressure filtration membrane. The fixed frame is slidably connected to the inside of the transparent container in the vertical direction and is in clearance fit with the transparent container. The linear driving member is electrically connected to the PLC control system.

[0014] By adopting the above technical solution, the PLC control system is used to control the linear driving member to drive the fixed frame to drive the transparent pressure filtration membrane to pressure-filter the mixed liquid in the transparent container, which can more conveniently separate the waste liquid and the white crystals, so that the white crystals stay between the bottom wall of the transparent container and the transparent pressure filtration membrane, facilitating the operator / automatically recycling the waste liquid obtained by pressure filtration without white crystals; at the same time, the transparent pressure filtration membrane has little influence on the irradiation light. As the transparent pressure filtration membrane lifts, its influence on the irradiation light can be roughly ignored, which is beneficial for the irradiation lamp and the imaging module to accurately identify and monitor whether there are white crystals in the mixed liquid.

[0015] Optionally, on any two opposite sides of the bottom wall of the transparent container, there are downwardly protruding material receiving grooves. A scraping device is provided in the transparent container for scraping the white crystals on the bottom wall of the transparent container into the material receiving grooves. The scraping direction of the scraping device is perpendicular to the extending direction of the material receiving grooves. The top of the material receiving groove and any one end of it are both open, and a plug is detachably and sealingly assembled at the opening of the end of the material receiving groove. A switch member for opening and closing the top opening of the material receiving groove is provided on the bottom wall of the transparent container.

[0016] By adopting the above technical solution, the operator can use the scraping device to scrape the white crystals after pressure filtration into the material receiving grooves for collection, and by controlling the switch member to open and close the top opening of the material receiving groove and controlling the plug to open and close the end opening of the material receiving groove, accordingly seal and close the channel between the bottom wall of the transparent container and the material receiving groove, and open the material receiving groove to discharge the white crystals that have been pressure filtered and accumulated on the bottom wall of the transparent container, so as to facilitate the continuous monitoring and identification inspection of the intermediate chloromethyl ethyl ether, primary amide and alkali solution mixture by the inspection device.

[0017] Optionally, the scraping device includes a scraping plate and a driving component for driving the scraping plate to reciprocate along a direction perpendicular to the extending direction of the material receiving groove. The scraping plate is slidably connected to the bottom wall of the transparent container, and the bottom wall of the scraping plate abuts against the bottom wall of the transparent container.

[0018] By adopting the above technical solution, using the driving component to drive the scraping plate to reciprocate along a direction perpendicular to the extending direction of the material receiving groove can more conveniently scrape the white crystals and a small amount of the mixed liquid accumulated between the bottom wall of the transparent container and the transparent pressure filtration membrane to the material receiving groove, realizing the collection and disposal of the white crystals.

[0019] Optionally, a plurality of vertical baffles are arranged in the transparent container in a staggered manner. One side of the baffle along its length direction is vertically fixedly connected to the side wall of the transparent container, and there is a gap between the other side and the side wall of the transparent container. A bent channel for the mixed liquid to pass through is formed between the plurality of baffles and the transparent container. The fixed frame is slidably connected to the baffle, and the outer side wall of the fixed frame is in clearance fit with the baffle.

[0020] By adopting the above technical solution, the bent channel formed between the plurality of vertical baffles and the transparent container for the mixed liquid to pass through can slow down the flow of the mixed liquid in the transparent container and block the white crystals in the mixed liquid to a certain extent, enabling the white crystals and the waste liquid to be more effectively separated.

[0021] Optionally, a material receiving box is detachably installed in the material receiving groove. The material receiving box has an upward opening, and the outer wall of the material receiving box is in clearance fit with the inner side wall of the material receiving groove.

[0022] By adopting the above technical solution, the material receiving box can sufficiently receive the white crystals falling into the material receiving groove. By closing the channel between the bottom of the transparent container and the top of the material receiving groove with the switch member, removing the plug at the end of the material receiving groove, and taking out the material receiving box from the material receiving groove, most of the white crystals falling into the material receiving groove can be taken away from the material receiving groove, reducing the residue of white crystals in the material receiving groove.

[0023] This application also provides an acetochlor production process, which is applied to the above-mentioned acetochlor production line and adopts the following technical solution:

[0024] An acetochlor production process includes the following steps:

[0025] Step 1: Pass HCL gas into the mixed solution of formaldehyde or paraformaldehyde and ethanol in the etherification reactor to prepare the intermediate chloromethyl ethyl ether.

[0026] Step 2: Pass an acylating agent into the acylation reactor to prepare a primary amide.

[0027] Step 3: Pass the above-prepared intermediate chloromethyl ethyl ether and primary amide into the lye in the condensation reactor, and control the temperature in the condensation reactor within the standard reaction temperature range to condense and prepare the crude acetochlor.

[0028] Step 4: While condensing and preparing the crude acetochlor, use the control module to control the first electromagnetic control valve to open, and the second and third electromagnetic control valves to close, and pass the mixed solution in the whole stage before, during, and after the condensation reaction into the transparent container. Use the imaging module to perform optical imaging on the mixed solution in the transparent container in real time to check whether white crystals appear in the mixed solution.

[0029] Step 5: When no white crystals appear in the mixed solution, use the control module to control the first and second electromagnetic control valves to open and the third electromagnetic control valve to close, and pass the prepared crude drug into the crude drug tank. When white crystals appear in the mixed solution, use the control module to control the first and third electromagnetic control valves to open and the second electromagnetic control valve to close, and use the pressure filtration device and the scraping device to filter and collect the waste liquid and white crystals.

[0030] Step 6: Adjust the temperature in the condensation reactor, the single addition amount of the primary amide, and the addition rate of the intermediate chloromethyl ethyl ether in real time according to the results in Step 5, and repeat the above steps.

[0031] Through the above technical solution,

[0032] In summary, this application includes at least one of the following beneficial technical effects:

[0033] 1. By arranging an inspection device between the condensation reactor and the crude drug tank, during the entire stage when the intermediate chloromethyl ethyl ether, primary amide, and lye are mixed in the condensation reactor and undergo a condensation reaction, continuously introduce into the transparent container the mixed solution of intermediate chloromethyl ethyl ether, primary amide, and lye at the beginning of mixing, during mixing / reacting, and after mixing / reacting, and use the irradiation lamp, imaging module, and control module to irradiate, obtain, and compare the optical imaging of the transparent container and the mixture inside the transparent container in real time, timely judge and identify whether white crystals are generated in the mixed solution, and control the on / off of the liquid path between the condensation reactor and the crude drug tank according to the real-time monitoring results, so that the operator can timely adjust reaction conditions such as the reaction temperature in the condensation reactor, the single-pass amount of primary amide, and the feeding rate of intermediate chloromethyl ethyl ether, effectively reducing production losses;

[0034] 2. By arranging a pressure filtration device and a scraping device inside the transparent container, when the imaging module monitors that there are white crystals in the transparent container, the operator can use the pressure filtration device to pressure-filter the mixed solution in the transparent container, separate most of the waste liquid from the white crystals, thereby discharge the white crystals that are pressure-filtered and accumulated on the bottom wall of the transparent container, and recycle the waste liquid obtained by pressure filtration that does not contain white crystals, so as to facilitate the continuous monitoring, identification, and inspection of the mixed solution of intermediate chloromethyl ethyl ether, primary amide, and lye by the inspection device;

[0035] 3. Through the cooperation of the transparent container, the receiving trough, the receiving box, the switch member, and the plug, the operator can more conveniently take most of the white crystals falling into the receiving trough away from the receiving trough, reducing the residue of white crystals in the receiving trough. Description of the Drawings

[0036] Figure 1 is the overall structural schematic diagram of the embodiment of the present application;

[0037] Figure 2 is the overall structural schematic diagram of the inspection device;

[0038] Figure 3 is the internal structural schematic diagram of the inspection device;

[0039] Figure 4 is the partial structural schematic diagram of the inspection device;

[0040] Figure 5 is related to Figure 4 the partial structural schematic diagram of the inspection device from different perspectives;

[0041] Figure 6 is the partial structural schematic diagram of the embodiment of the present application made to show the cooperation relationship between the scraper and the drive shaft.

[0042] Reference signs: 1, condensation reactor; 2, crude drug tank; 3, waste liquid tank; 4, inspection device; 41, transparent container; 411, liquid inlet pipe; 412, crude drug discharge pipe; 413, waste liquid discharge pipe; 414, material receiving tank; 415, plug; 416, switch member; 417, baffle; 42, irradiation lamp; 5, pressure filtration device; 51, fixed frame; 511, pressing plate; 52, transparent pressure filtration membrane; 53, linear driving member; 6, scraping device; 61, scraper; 611, positioning rib; 612, clamping projection; 613, bearing strip; 62, driving assembly; 621, rodless cylinder; 622, sliding seat; 623, driving shaft; 6231, positioning groove; 6232, clamping groove. Detailed implementation manners

[0043] The following further describes the present application in detail with reference to Figures 1-6 the accompanying drawings.

[0044] An embodiment of the present application discloses an acetochlor production line.

[0045] Referring to Figure 1 , an acetochlor production line includes a raw material tank, an etherification reactor for preparing an intermediate chloromethyl ethyl ether solution, an acylation reactor for preparing a primary amide, a condensation reactor 1 for carrying out a condensation reaction of the intermediate chloromethyl ethyl ether, the primary amide and an alkali solution therein, a crude drug tank 2 for temporarily storing acetochlor crude drug, and pipelines for connecting the above tanks and each reactor according to the production process; wherein, the liquid outlet ends of the etherification reactor and the acylation reactor are both connected to the liquid inlet end of the condensation reactor 1 through pipelines, and an inspection device 4 is provided between the condensation reactor 1 and the crude drug tank 2. The inspection device 4 is used to monitor the mixing liquid condition in the condensation reactor 1 during the whole stage of the mixing and condensation reaction of the intermediate chloromethyl ethyl ether, the primary amide and the alkali solution in the condensation reactor 1, and control the on-off of the liquid path between the condensation reactor 1 and the crude drug tank 2 according to the real-time monitoring results.

[0046] Specifically, the inspection device 4 includes a transparent container 41 communicated between the condensation reactor 1 and the crude drug tank 2, an irradiation lamp 42 and an imaging module for obtaining and comparing the imaging of the mixing liquid in the transparent container 41, and a control module for controlling the liquid inlet and outlet of the transparent container 41 according to the imaging of the imaging module.

[0047] Referring to Figure 1 and Figure 2, the transparent container 41 is a rectangular box. Liquid inlet and outlet are respectively provided on two opposite side walls of the transparent container 41 along its length direction. A liquid inlet pipe 411 for connecting the condensation reactor 1 and the transparent container 41 is connected to the liquid inlet of the transparent container 41. A crude drug discharge pipe 412 and a waste liquid discharge pipe 413 are simultaneously connected to the liquid outlet of the transparent container 41. The crude drug discharge pipe 412 is used to connect the transparent container 41 and the crude drug tank 2. One end of the waste liquid discharge pipe 413 far from the transparent container 41 is connected to a waste liquid tank 3; the control module includes a first electromagnetic control valve, a second electromagnetic control valve and a third electromagnetic control valve respectively provided on the liquid inlet pipe 411, the crude drug discharge pipe 412 and the waste liquid discharge pipe 413, and a PLC control system for controlling the first electromagnetic control valve, the second electromagnetic control valve and the third electromagnetic control valve. The first electromagnetic control valve, the second electromagnetic control valve and the third electromagnetic control valve are respectively used to control the on-off and flow rate of the liquid paths of the liquid inlet pipe 411, the crude drug discharge pipe 412 and the waste liquid discharge pipe 413, and the PLC control system is electrically connected to the imaging module.

[0048] The irradiation lamp 42 is arranged directly above the transparent container 41 and is used to continuously irradiate the transparent container 41 from top to bottom. The imaging module includes a substrate arranged directly below the transparent container 41, and an optical imaging instrument, a display control terminal and related integrated circuits which are electrically connected to the substrate and used for imaging processing; the imaging image of the mixed liquid that meets the standard and does not contain white crystals is pre-stored in the display control terminal. The irradiation lamp 42 is used to irradiate the transparent container 41 in real time. At the same time, the optical imaging instrument is used to perform stroboscopic shooting on the imaging of the transparent container 41 and the mixed liquid in the transparent container 41 on the substrate every 10 - 30 minutes, and send the stroboscopic shooting image information to the display control terminal. At the display control terminal, the real-time stroboscopic shooting image information is compared with the pre-stored standard imaging image to identify and judge in real time whether there are white crystals in the mixed liquid of intermediate chloromethyl ether, primary amide and lye in the transparent container 41 at the beginning of mixing, during mixing / reaction, and after mixing / reaction.

[0049] Refer to Figure 2 and Figure 3 , when there are white crystals in the transparent container 41, the PLC control system can correspondingly control the first electromagnetic control valve to keep the liquid inlet pipe 411 open, control the second electromagnetic control valve to close the crude drug discharge pipe 412, and control the third electromagnetic control valve to close the waste liquid discharge pipe 413, so as to discard and recycle the mixed liquid in the transparent container 41; correspondingly, a pressure filtration device 5 for pressure-filtering the white crystals in the waste liquid from top to bottom when there are white crystals in the transparent container 41, a material receiving tank 414 for recycling the white crystals and a scraping device 6 are arranged in the transparent container 41.

[0050] The filter press device 5 includes a fixed frame 51 slidably connected in the transparent container 41 in the vertical direction, a transparent filter membrane 52 detachably and fixedly installed in the fixed frame 51, and a linear drive member 53 for driving the fixed frame 51 to linearly lift and lower in the vertical direction.

[0051] Specifically, referring to Figure 3 and Figure 4 , a plurality of mutually parallel, vertical baffles 417 are staggered at the upper part of the transparent container 41. The baffles 417 are parallel to the side walls corresponding to the wide sides of the transparent container 41. One side of the baffle 417 along its length direction is perpendicularly and fixedly connected to the side wall of the transparent container 41, and there is a gap between the other side and the side wall of the transparent container 41. There is a gap between the bottom surface of the lower side of the baffle 417 and the bottom wall of the transparent container 41. A bent channel through which the mixed liquid can pass is formed between the plurality of baffles 417 and the transparent container 41. The liquid inlet of the transparent container 41 is located below the baffle 417, and the liquid outlet is located above the baffle 417.

[0052] The fixed frame 51 is a special-shaped frame. A plurality of micropores are formed through the transparent filter membrane 52. The fixed frame 51 is slidably connected to the baffle 417, and the outer side wall of the fixed frame 51 is in clearance fit with the baffle 417 and the inner side wall of the transparent container 41. The linear drive member 53 is preferably a cylinder in the embodiment of the present application, and can also be a push rod motor or a screw motor in other application embodiments. The linear drive member 53 is electrically connected to the PLC control system. At least two groups of linear drive members 53 are provided in the embodiment of the present application, and the linear drive members 53 are evenly arranged at the corners of the transparent container 41. The fixed frame 51 is vertically and fixedly connected to the end of the output shaft of the linear drive member 53. The operator can conveniently drive the fixed frame 51 to drive the transparent filter membrane 52 to lift and lower vertically by controlling the linear drive member 53 through the PLC control system. When the bottom surface of the transparent filter membrane 52 moves to be flush with the bottom surface of the baffle 417, the transparent filter membrane 52 no longer moves downward.

[0053] Referring to Figure 3 and Figure 4, there are two material receiving grooves 414 opened on the bottom wall of the transparent container 41. The two material receiving grooves 414 have the same specifications and are respectively oppositely opened at both side edges of the bottom wall of the transparent container 41 along its width direction. The material receiving grooves 414 protrude downward on the bottom wall of the transparent container 41. The top and any one end of the material receiving grooves 414 are both open, and the top of the material receiving grooves 414 is communicated with the inner cavity of the transparent container 41; a flexible plug 415 is detachably and hermetically assembled at the opening of the end of the material receiving groove 414. A material receiving box with an upward opening is detachably installed in the material receiving groove 414. The specification of the material receiving box is adapted to that of the material receiving groove 414, and the outer wall of the material receiving box is in clearance fit with the inner side wall of the transparent container 41 at the position of the material receiving groove 414. A switch member 416 for opening and closing the top opening of the material receiving groove 414 is also provided on the bottom wall of the transparent container 41; in the embodiment of the present application, the switch member 416 is specifically a switch valve plate that horizontally moves along the bottom wall of the transparent container 41 and opens and closes the channel between the transparent container 41 and the material receiving groove 414. The switch member 416 can be manually opened and closed or be opened and closed under the control of the PLC control system.

[0054] Referring to Figure 4 and Figure 5 , the scraping device 6 includes a scraping plate 61 slidably connected above the bottom wall of the transparent container 41 and a driving assembly 62 for driving the scraping plate 61 to reciprocally slide along a direction perpendicular to the extending direction of the material receiving groove 414.

[0055] Specifically, the driving assembly 62 includes a rodless cylinder 621, a sliding seat 622 slidably assembled on the rodless cylinder 621, and a driving shaft 623 fixedly installed on the sliding seat 622. The length direction of the output shaft of the rodless cylinder 621 is consistent with the width direction of the transparent container 41; the sliding seat 622 is sleeved on the output shaft of the rodless cylinder 621 and slides along the length extending direction of the output shaft of the rodless cylinder 621; the driving shaft 623 is in the shape of a round rod, and the driving shaft 623 is parallel to the bottom wall of the transparent container 41 and perpendicular to the output shaft of the rodless cylinder 621.

[0056] Referring to Figure 5 and Figure 6 , the scraping plate 61 is parallel to the driving shaft 623, and the scraping plate 61 specifically includes an integrally formed fan-shaped part and a pointed part. Both the fan-shaped part and the pointed part are symmetrically arranged about the midline of the scraping plate 61. The outer arc of the fan-shaped part of the scraping plate 61 is a major arc, and the tip of the pointed part faces outward; the fan-shaped part is coaxially sleeved and rotatably connected to the driving shaft 623 along its axis. A positioning rib 611, a clamping convex block 612, a positioning groove 6231, and a clamping groove 6232 are provided between the middle of the driving shaft 623 and the inner side of the fan-shaped part for limiting the rotation of the fan-shaped part; when the fan-shaped part rotates to the end point of its rotation, the tip edge of the pointed part is adapted to be in movable contact with the bottom wall of the transparent container 41 in the horizontal direction, and the upper side of the fan-shaped part is in movable contact with the lower surface of the baffle 417.

[0057] Specifically, the positioning groove 6231 is a sector-shaped groove coaxially opened in the middle of the driving shaft 623. The positioning rib 611 is a triangular rib protruding from the middle of the sector part. The positioning rib 611 is also symmetric about the midline of the scraping plate 61. And the positioning rib 611 is slidably connected in the positioning groove 6231 along the circumferential direction of the driving shaft 623. The two side edges of the positioning rib 611 along the circumferential direction of the driving shaft 623 are respectively in movable contact with the two inner side walls of the driving shaft 623 corresponding to the positioning groove 6231 in the circumferential direction; there are two groups of clamping protrusions 612. The number of each group of clamping protrusions 612 includes several, and the clamping protrusions 612 are elastic blocks. The two groups of clamping protrusions 612 are respectively protruding from the two side edges of the positioning rib 611 along the circumferential direction of the driving shaft 623. The clamping grooves 6232 are correspondingly opened on the two inner side walls of the driving shaft 623 corresponding to the positioning groove 6231 in the circumferential direction. And the clamping grooves 6232 communicate with the positioning groove 6231. The number and position of the clamping grooves 6232 are arranged in one-to-one correspondence with the number and position of the clamping protrusions 612. And the corresponding clamping protrusions 612 and clamping grooves 6232 are cooperatively clamped to realize the clamping and fixing of the scraping plate 61 and the driving shaft 623 when the scraping plate 61 rotates to its two rotation end points.

[0058] Further, referring to Figure 5 and Figure 6 As shown in FIGS. 5 and 6, the lower parts of the two side edges of the fixed frame 51 along the width direction of the transparent container 41 protrude downward to form pressing plates 511. Two pressure-bearing strips 613 are protrudingly arranged on the outer side of the sector part of the scraping plate 61 for the pressing plates 511 to press down the scraping plate 61 downward and enable the scraping plate 61 to rotate.

[0059] The two pressure-bearing strips 613 are also symmetric with respect to the midline of the scraping plate 61. When the scraping plate 61 slides to its sliding end point along with the rodless cylinder 621, the scraping plate 61 is located above any one of the material receiving grooves 414. By using the linear driving member 53 to drive the fixed frame 51 and the transparent filter membrane 52 to move downward, the pressing plate 511 below the fixed frame 51 can press down the pressure-bearing strip 613 on the upper part of the scraping plate 61 and drive the scraping plate 61 to rotate around the driving shaft 623; and when the linear driving member 53 drives the fixed frame 51 to move until the bottom surface of the transparent filter membrane 52 is flush with the lower surface of the baffle 417, the pressing plate 511 no longer presses down the pressure-bearing strip 613, and the positioning rib 611 is switched from being in contact with the inner side wall of the driving shaft 623 corresponding to the positioning groove 6231 on its left / right side to being in contact with the inner side wall of the driving shaft 623 corresponding to the positioning groove 6231 on its right / left side. The corresponding clamping protrusions 612 and clamping grooves 6232 are clamped at this time, that is, the scraping plate 61 rotates from one rotation end point to the other rotation end point. And after the scraping plate 61 rotates to its rotation end point, it remains fixed to the driving shaft 623 without external force influence.

[0060] When the imaging module detects the presence of white crystals in the transparent container 41, the operator can first control the opening and closing of the liquid inlet and outlet of the transparent container 41, and use the linear drive member 53 to drive the fixed frame 51 and the transparent filter membrane 52 to slide downward, filter the mixed liquid in the transparent container 41, and separate most of the waste liquid from the white crystals, so that the white crystals stay below the transparent filter membrane 52 and most of the waste liquid is filtered to above the transparent filter membrane; and during this process, the operator can control the scraper 61 to scrape the white crystals and a small amount of waste liquid between the transparent filter membrane 52 and the bottom wall of the transparent container 41. As the scraper 61 slides, the waste liquid located at the sliding front end of the scraper 61 can be further filtered to above the transparent filter membrane 52, further realizing the separation of the white crystals and the waste liquid, so that the white crystals are filtered to above the material receiving groove 414 and fall into the material receiving box; correspondingly, after the white crystals fall into the material receiving box, the switch member 416 is used to close the channel between the bottom of the transparent container 41 and the top of the material receiving groove 414, remove the plug 415 at the end of the material receiving groove 414, and take out the material receiving box from the material receiving groove 414, which can take most of the white crystals falling into the material receiving groove 414 away from the material receiving groove 414, reduce the white crystal residue in the material receiving groove 414, and is beneficial for the operator to recycle the filtered waste liquid without white crystals, so as to realize the continuous monitoring and identification test of the intermediate chloromethyl ethyl ether, primary amide and lye mixed liquid by the inspection device 4.

[0061] The implementation principle of an acetochlor production line in an embodiment of this application is as follows: By arranging an inspection device 4 between the condensation reaction kettle 1 and the technical material tank 2, during the entire stage when the intermediate chloromethyl ethyl ether, primary amide, and lye are mixed and undergo a condensation reaction in the condensation reaction kettle 1, the mixture of the initially mixed, mixed / reacting, and post-mixed / post-reacted intermediate chloromethyl ethyl ether, primary amide, and lye is continuously introduced into the transparent container 41, and the irradiation lamp 42, imaging module, and control module are used to irradiate, obtain, and compare the optical imaging of the transparent container 41 and the mixture inside the transparent container 41 in real time, so as to timely judge and identify whether white crystals are generated in the mixed liquid; According to the real-time monitoring results, the operator can correspondingly control the on / off of the liquid paths between the condensation reaction kettle 1 and the transparent container 41, between the transparent container 41 and the technical material tank 2, and between the transparent container 41 and the waste liquid tank 3 by using the first electromagnetic control valve, the second electromagnetic control valve, and the third electromagnetic control valve, and timely adjust the reaction conditions such as the reaction temperature in the condensation reaction kettle 1, the single-pass amount of primary amide, and the feeding speed of the intermediate chloromethyl ethyl ether, effectively reducing production losses; At the same time, when the imaging module monitors that there are white crystals in the transparent container 41, the operator can also use the pressure filtration device 5, the scraping device 6, the material receiving tank 414, and the material receiving box to perform pressure filtration on the mixed liquid in the transparent container 41, separate most of the waste liquid from the white crystals, discharge the white crystals that are pressure-filtered and accumulated on the bottom wall of the transparent container 41, and recycle the waste liquid obtained by pressure filtration that does not contain white crystals to ensure the continuous monitoring, identification, and inspection of the mixture of the intermediate chloromethyl ethyl ether, primary amide, and lye by the inspection device 4, further reducing production losses.

[0062] Another aspect of the embodiment of this application is to disclose an acetochlor production process, which is applied to the acetochlor production line described above, and includes the following steps:

[0063] Step 1: Introduce HCL gas into the mixed liquid of formaldehyde or paraformaldehyde and ethanol in the etherification reaction kettle to prepare the intermediate chloromethyl ethyl ether;

[0064] Step 2: Introduce an acylating agent into the acylation reaction kettle to prepare the primary amide;

[0065] Step 3: Introduce the intermediate chloromethyl ethyl ether and primary amide prepared in Step 1 and Step 2 into the lye in the condensation reaction kettle 1, and control the temperature in the condensation reaction kettle 1 within the standard reaction temperature range to condense and prepare the acetochlor technical material;

[0066] Step 4: While condensing to prepare the acetochlor technical, use the control module to control the first solenoid valve to open, and the second and third solenoid valves to close, and introduce the mixed liquid in the whole stage before, during, and after the condensation reaction into the transparent container 41. Use the imaging module to perform optical imaging on the mixed liquid in the transparent container 41 in real time to check whether white crystals appear in the mixed liquid;

[0067] Step 5: When no white crystals appear in the mixed liquid, use the control module to control the first and second solenoid valves to open, and the third solenoid valve to close, and introduce the prepared technical into the technical tank 2; when white crystals appear in the mixed liquid, use the control module to control the first and third solenoid valves to open, and the second solenoid valve to close, and use the pressure filtration device 5 and the scraping device 6 to filter and collect the waste liquid and white crystals;

[0068] Step 6: Adjust the temperature in the condensation reactor 1, the single addition amount of the primary amide, and the addition rate of the intermediate chloromethyl ethyl ether in real time according to the results in Step 5, and repeat the above steps.

[0069] The above are all preferred embodiments of the present application, and do not limit the protection scope of the present application accordingly. Therefore, all equivalent changes made according to the structure, shape, and principle of the present application should be covered within the protection scope of the present application.

Claims

1. An acetochlor production line, characterized in that: It includes a raw material tank, an etherification reactor, an acylation reactor, a condensation reactor (1), and a technical drug tank (2) that are connected in sequence through pipelines. The condensation reactor (1) is used for the condensation reaction of intermediate chloromethyl ethyl ether, primary amide, and lye therein. The technical drug tank (2) is used for temporarily storing acetochlor technical drug. An inspection device (4) is provided between the condensation reactor (1) and the technical drug tank (2); the inspection device (4) includes: A transparent container (41) connected between the condensation reactor (1) and the technical drug tank (2); An irradiation lamp (42) and an imaging module for obtaining and comparing the imaging of the mixed liquid in the transparent container (41). The irradiation lamp (42) is arranged above the transparent container (41), and the imaging part of the imaging module is located below the transparent container (41). And a standard imaging image of the qualified mixed liquid is preset in the imaging module; And a control module for controlling the inflow and outflow of the transparent container (41) according to the imaging of the imaging module; An inlet pipe (411) connecting the condensation reactor (1) and the transparent container (41), a technical drug discharge pipe (412) connecting the transparent container (41) and the technical drug tank (2), and a waste liquid discharge pipe (413) are provided on the transparent container (41). The waste liquid discharge pipe (413) is connected to a waste liquid tank (3); the control module includes a first electromagnetic control valve, a second electromagnetic control valve, and a third electromagnetic control valve respectively arranged on the inlet pipe (411), the technical drug discharge pipe (412), and the waste liquid discharge pipe (413), and a PLC control system for controlling the first electromagnetic control valve, the second electromagnetic control valve, and the third electromagnetic control valve. The PLC control system is electrically connected to the imaging module; The top wall and the bottom wall of the transparent container (41) are both horizontally arranged. A pressure filtration device (5) is provided in the transparent container (41) for pressing and filtering the white crystals in the waste liquid from top to bottom when there are white crystals in the transparent container (41).

2. The acetochlor production line according to claim 1, wherein: The pressure filtration device (5) includes a fixed frame (51), a transparent pressure filtration membrane (52) arranged in the fixed frame (51), and a linear driving member (53) for driving the fixed frame (51) to move up and down. A plurality of micropores are formed through the transparent pressure filtration membrane (52). The fixed frame (51) is slidably connected to the inside of the transparent container (41) in the vertical direction and is in clearance fit with the transparent container (41). The linear driving member (53) is electrically connected to the PLC control system.

3. The acetochlor production line according to claim 2, characterized in that: On any two opposite sides of the bottom wall of the transparent container (41), there are downwardly protruding material receiving grooves (414). A scraping device (6) is provided in the transparent container (41) for scraping the white crystals on the bottom wall of the transparent container (41) into the material receiving grooves (414). The scraping direction of the scraping device (6) is perpendicular to the extending direction of the material receiving grooves (414). The top of the material receiving grooves (414) and the end of any one of its ends are both open, and a plug (415) is detachably and sealingly assembled at the opening of the end of the material receiving grooves (414). A switch member (416) for opening and closing the top opening of the material receiving grooves (414) is provided on the bottom wall of the transparent container (41).

4. The acetochlor production line according to claim 3, wherein: The scraping device (6) includes a scraping plate (61) and a driving assembly (62) for driving the scraping plate (61) to reciprocate along a direction perpendicular to the extending direction of the material receiving grooves (414). The scraping plate (61) is slidably connected to the bottom wall of the transparent container (41), and the bottom wall of the scraping plate (61) abuts against the bottom wall of the transparent container (41).

5. The acetochlor production line according to claim 2, wherein: A plurality of vertical baffles (417) are staggered in the transparent container (41). One side of the baffle (417) along its length direction is vertically fixedly connected to the side wall of the transparent container (41), and there is a gap between the other side and the side wall of the transparent container (41). A bent channel through which the mixed liquid can pass is formed between the plurality of baffles (417) and the transparent container (41). The fixed frame (51) is slidably connected to the baffle (417), and the outer side wall of the fixed frame (51) is in clearance fit with the baffle (417).

6. The acetochlor production line according to claim 3, characterized in that: A receiving box is detachably installed in the material receiving grooves (414). The receiving box has an upward opening, and the outer wall of the receiving box is in clearance fit with the inner side wall of the material receiving grooves (414).

7. A production process of acetochlor, applied to the acetochlor production line described in any one of claims 1-6, characterized in that: Including the following steps: Step 1: Pass HCL gas into formaldehyde, or a mixed liquid of paraformaldehyde and ethanol in an etherification reactor to prepare the intermediate chloromethyl ethyl ether; Step 2: Pass an acylating agent into an acylation reactor to prepare a primary amide; Step 3: Pass the intermediate chloromethyl ethyl ether and the primary amide prepared in Step 1 and Step 2 into the lye in the condensation reactor (1), and control the temperature in the condensation reactor (1) within the standard reaction temperature range to condense and prepare the technical herbicide acetochlor; Step 4: While condensing and preparing the technical herbicide acetochlor, use the control module to control the first solenoid valve to open, and the second solenoid valve and the third solenoid valve to close, and pass the mixed liquid in all stages before, during, and after the condensation reaction into the transparent container (41). The imaging module performs optical imaging on the mixed liquid in the transparent container (41) in real time to check whether white crystals appear in the mixed liquid; Step Five: When no white crystals appear in the mixed solution, use the control module to control the opening of the first solenoid valve and the second solenoid valve and the closing of the third solenoid valve, and introduce the prepared crude drug into the crude drug tank (2); when white crystals appear in the mixed solution, use the control module to control the opening of the first solenoid valve and the third solenoid valve and the closing of the second solenoid valve, and use the pressure filtration device (5) and the scraping device (6) to filter and collect the waste liquid and white crystals; Step Six: According to the results in Step Five, adjust the temperature in the condensation reactor (1), the single addition amount of the primary amide, and the addition rate of the intermediate chloromethyl ethyl ether in real time, and repeat the above steps.

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