CN113578218A - Multi-step integrated device for preparing buprofezin and preparation method thereof - Google Patents

Multi-step integrated device for preparing buprofezin and preparation method thereof Download PDF

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Publication number
CN113578218A
CN113578218A CN202110775264.4A CN202110775264A CN113578218A CN 113578218 A CN113578218 A CN 113578218A CN 202110775264 A CN202110775264 A CN 202110775264A CN 113578218 A CN113578218 A CN 113578218A
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China
Prior art keywords
liquid
reaction
box
buprofezin
pivot
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CN202110775264.4A
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Chinese (zh)
Inventor
潘荣欢
张孝国
朱光文
李健
黄显超
寿王鸽
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Anhui Guangxin Agrochemcial Co Ltd
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Anhui Guangxin Agrochemcial Co Ltd
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Priority to CN202110775264.4A priority Critical patent/CN113578218A/en
Publication of CN113578218A publication Critical patent/CN113578218A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/245—Stationary reactors without moving elements inside placed in series
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C331/00—Derivatives of thiocyanic acid or of isothiocyanic acid
    • C07C331/16—Isothiocyanates
    • C07C331/18—Isothiocyanates having isothiocyanate groups bound to acyclic carbon atoms
    • C07C331/20—Isothiocyanates having isothiocyanate groups bound to acyclic carbon atoms of a saturated carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D285/00—Heterocyclic compounds containing rings having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by groups C07D275/00 - C07D283/00
    • C07D285/15—Six-membered rings
    • C07D285/16—Thiadiazines; Hydrogenated thiadiazines
    • C07D285/34—1,3,5-Thiadiazines; Hydrogenated 1,3,5-thiadiazines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/005—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/00033—Continuous processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00092—Tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00164—Controlling or regulating processes controlling the flow

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a multi-step integrated device for preparing buprofezin and a preparation method thereof, relates to the technical field of buprofezin preparation, and aims to solve the problems that the conventional buprofezin needs multiple steps in the production process, needs multiple devices, is difficult to operate and is not convenient for standardized and rapid production. The utility model discloses a liquid injection device, including main body support, mounting panel, liquid suction cylinder, liquid pump, main body support's upper end is installed upper portion support, the mounting panel is all installed to the both sides of main body support upper end, the internally mounted of main body support has the pivot, the inside of pivot is provided with divides the liquid pipe, one side that the pivot was kept away from to the mounting panel is installed and is divided the liquid cylinder, divide the liquid cylinder to be close to one side of pivot and install the push pedal, the internally mounted of push pedal has liquid suction flexible hose, liquid suction flexible hose keeps away from the one end of pivot and installs the liquid pump of dividing, divide the liquid pump to keep away from the one end of pivot and install the notes liquid pipe.

Description

Multi-step integrated device for preparing buprofezin and preparation method thereof
Technical Field
The invention relates to the technical field of buprofezin preparation, in particular to a multi-step integrated device for buprofezin preparation and a preparation method thereof.
Background
Buprofezin, also known as "delphacidofol", belongs to the class of insecticides of insect growth regulators. The insecticidal composition is mainly used for controlling pests of crops such as rice, fruit trees, tea trees, vegetables and the like, and has lasting larvicidal activity on coleoptera, partial homoptera and acarina. Can effectively prevent and treat the rice from the cicada and the plant hopper: cicadae on potato; whitefly family on citrus, cotton and vegetables; the pesticide is used for large-area spraying of agricultural pesticides in the families of coccidae, pelagidae and mealybug on citrus, can cause direct pollution of soil and certain pollution to water, can cause pesticide residue on crops after long-term use, has no more research on the action mechanism of buprofezin on human bodies, mainly acts on the neuroendocrine system of insects through different drug-receiving parts to interfere the normal activities of the ventral cardiotrophism, the precordial gland and the like, and presents a series of adverse reactions.
However, the conventional buprofezin involves more steps in the production process, wherein tert-butyl isothiocyanate needs to be prepared firstly, and various devices are needed in the process, so that the operation difficulty is high, and the standardized and rapid production is not convenient; therefore, the existing requirements are not met, and a multi-step integrated device for preparing buprofezin and a preparation method thereof are provided for the device.
Disclosure of Invention
The invention aims to provide a multi-step integrated device for preparing buprofezin and a preparation method thereof, and aims to solve the problems that the buprofezin provided in the background art needs multiple steps in the production process, needs multiple devices, is difficult to operate and is not convenient for standardization and rapid production.
In order to achieve the purpose, the invention provides the following technical scheme: a multi-step integrated device for preparing buprofezin comprises a main body bracket, an upper bracket is arranged at the upper end of the main body bracket, the two sides of the upper end of the main body bracket are both provided with mounting plates, the inside of the main body bracket is provided with a rotating shaft, a liquid separating pipe is arranged inside the rotating shaft, a liquid separating cylinder is arranged on one side of the mounting plate away from the rotating shaft, a push plate is arranged on one side of the liquid separating cylinder close to the rotating shaft, a liquid absorbing elastic hose is arranged inside the push plate, a liquid separating pump is arranged at one end of the liquid absorbing elastic hose far away from the rotating shaft, a liquid injecting pipe is arranged at one end of the liquid separating pump far away from the rotating shaft, stirring fan blades are arranged outside the rotating shaft, a raw material primary treatment box is arranged at the upper end inside the main body bracket, the liquid separation adjusting washing box is installed below the raw material primary treatment box, and a treatment heat exchange tube is installed outside the raw material primary treatment box.
Preferably, a water storage tank is installed on one side of the lower end in the main body support, the water storage tank is fixedly connected with the main body support, a cleaning pump is installed below the water storage tank, the cleaning pump is connected with the water storage tank through a pipeline, a cleaning pipeline is installed on one side, close to the rotating shaft, of the cleaning pump, and the cleaning pipeline is fixedly connected with the cleaning pump.
Preferably, a liquid transfer pipe is installed on one side of the lower end of the liquid separation adjusting washing box, a backflow reaction kettle is installed at the lower end of the liquid transfer pipe, an evaporation heat exchange pipe is installed outside the backflow reaction kettle, and the evaporation heat exchange pipe is fixedly connected with the backflow reaction kettle through a clamping groove.
Preferably, the division board is installed to backward flow reation kettle's lower extreme, division board and backward flow reation kettle fixed connection, the reaction box is installed to the lower extreme of division board, reaction box and division board fixed connection, the externally mounted of reaction box has the reaction heat exchange tube, the reaction heat exchange tube passes through draw-in groove fixed connection with the reaction box.
Preferably, the material box is installed to the inside lower extreme of main part support, material box and main part support pass through draw-in groove sliding connection.
Preferably, the upper end in the material box is provided with a filter basket, and the filter basket is connected with the material box through a clamping groove.
Preferably, divide the liquid and adjust the lower extreme of washing case and install the discharge pipe way, the discharge pipe way with divide the equal fixed connection of liquid regulation washing case and main part support, firm support is installed to the lower extreme of main part support, agitator motor is installed to the upper end of upper portion support, agitator motor passes through the coupling joint with the pivot.
A preparation method of a multi-step integrated device for preparing buprofezin comprises the following steps:
the method comprises the following steps: the method comprises the following steps that a worker adds raw materials and water into a raw material primary treatment box, then a stirring motor is powered on to drive a rotating shaft to rotate, so that stirring blades stir materials to fully dissolve the materials, then a treatment heat exchange tube is used for heating a material solution, a certain amount of hydrochloric acid is dripped, heat is preserved for four hours, the stirring motor is powered off after a period of reaction time, the treatment heat exchange tube is used for cooling the material solution, and the material solution is layered;
step two: the liquid separation cylinder extends to push the push plate to move, so that the liquid absorption elastic hose is in contact with the liquid separation pipe, and then the liquid separation pump pumps the layered liquid into the liquid separation regulation washing box;
step three: adding an alkaline aqueous solution into an upper oil layer obtained after liquid separation in a liquid separation regulation washing tank, washing, regulating the pH value of a material by washing to 6.8-7.2, then feeding the material into a reflux reaction kettle through a pipette, heating the material by an evaporation heat exchange tube, refluxing the material until water is absent to obtain light yellow transparent liquid, collecting the separated water in a water storage tank, feeding the material into the reaction tank, adding a catalyst into the reaction tank by a worker, increasing the temperature of the material and the catalyst by the reaction heat exchange tube, and carrying out heat preservation reaction for six hours;
step four: after reacting for a period of time, discharging the product into a material box, and filtering out insoluble substances in the product by using a filter basket.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the liquid separation pipe is arranged in the rotating shaft, so that the liquid separation treatment can be carried out on the layered liquid in the raw material primary treatment box under the condition that the rotating shaft drives the stirring fan blades to rotate without influencing the liquid transfer, the liquid separation can be directly carried out without carrying out liquid transfer, the operation steps are reduced, the production efficiency is increased greatly, the loss of materials during liquid transfer is avoided, the waste is avoided, the use effect of the device is increased, the liquid absorption elastic hose is arranged to be matched with the liquid separation cylinder to be communicated with the liquid separation pipe, the liquid separation pump can conveniently absorb the layered liquid in the device, and the practicability of the device is increased;
2. according to the invention, the water storage tank is arranged to collect distilled water, so that the distilled water can be washed by matching with the cleaning pump, the practicability of the device is increased, the waste is avoided, the use cost of the device is reduced, the filter basket is arranged at the upper end of the material tank, insoluble substances can be quickly filtered, the product is quickly obtained, meanwhile, the insoluble substances can be conveniently removed by workers, the device is more convenient to use, and the working difficulty of the workers is reduced.
Drawings
FIG. 1 is a three-dimensional perspective view of a multi-step integrated apparatus for buprofezin preparation according to the present invention;
FIG. 2 is a schematic structural diagram of a multi-step integrated apparatus for buprofezin preparation according to the present invention;
FIG. 3 is an enlarged view of a portion A of the present invention;
FIG. 4 is an enlarged view of a portion B of the present invention;
FIG. 5 is an enlarged view of a portion C of the present invention.
In the figure: 1. a main body support; 2. an upper bracket; 3. a stirring motor; 4. a material box; 5. mounting a plate; 6. a liquid separating cylinder; 7. pushing the plate; 8. a liquid separating pump; 9. a liquid-absorbing elastic hose; 10. a liquid injection pipe; 11. a liquid separation adjusting washing box; 12. a pipette; 13. refluxing the reaction kettle; 14. an evaporation heat exchange pipe; 15. a partition plate; 16. a reaction box; 17. a reaction heat exchange pipe; 18. a stabilizing bracket; 19. a filter basket; 20. a raw material primary treatment box; 21. processing the heat exchange pipe; 22. a discharge conduit; 23. a stirring fan blade; 24. a rotating shaft; 25. a liquid separating pipe; 26. cleaning the pump; 27. a water storage tank; 28. and (5) cleaning the pipeline.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1-5, an embodiment of the present invention is shown: a multi-step integrated device for preparing buprofezin comprises a main body support 1, an upper support 2 is installed at the upper end of the main body support 1, mounting plates 5 are installed on two sides of the upper end of the main body support 1, a rotating shaft 24 is installed inside the main body support 1, the rotating shaft 24 is connected with the main body support 1 and the upper support 2 through bearings, a liquid distribution pipe 25 is arranged inside the rotating shaft 24, the liquid distribution pipe 25 is arranged inside the rotating shaft 24, liquid distribution treatment can be carried out on layered liquid inside a raw material primary treatment box 20 under the condition that the rotating shaft 24 drives a stirring fan blade 23 to rotate without influencing, liquid distribution can be directly carried out without liquid transfer, operation steps are reduced, production efficiency is increased greatly, loss of materials during liquid transfer is avoided, waste is avoided, the use effect of the device is improved, the liquid distribution pipe 25 is fixedly connected with the rotating shaft 24, a liquid distribution cylinder 6 is installed on one side, far away from the rotating shaft 24, of the mounting plates 5, one side of the liquid separating cylinder 6 close to the rotating shaft 24 is provided with a push plate 7, the push plate 7 is internally provided with an imbibition elastic hose 9, the imbibition elastic hose 9 is arranged to be matched with the liquid separating cylinder 6 to be communicated with a liquid separating pipe 25, so that the liquid separating pump 8 can absorb the layered liquid in the device, the practicability of the device is improved, the imbibition elastic hose 9 is fixedly connected with the push plate 7, one end of the imbibition elastic hose 9 far away from the rotating shaft 24 is provided with a liquid separating pump 8, the liquid separating pump 8 is fixedly connected with the main body support 1, one end of the liquid separating pump 8 far away from the rotating shaft 24 is provided with a liquid injecting pipe 10, the outer part of the rotating shaft 24 is provided with a stirring fan blade 23, the stirring fan blade 23 is fixedly connected with the rotating shaft 24, the upper end in the main body support 1 is provided with a raw material primary treatment box 20, the raw material primary treatment box 20 is fixedly connected with the main body support 1, and a liquid separating regulation washing box 11 is arranged below the raw material primary treatment box 20, divide liquid to adjust washing case 11 and main part support 1 fixed connection, annotate the lower extreme of liquid pipe 10 and divide liquid to adjust washing case 11 fixed connection, the externally mounted of raw materials preliminary treatment case 20 has the processing heat exchange tube 21.
Further, a water storage tank 27 is installed on one side of the inner lower end of the main body support 1, the water storage tank 27 is fixedly connected with the main body support 1, a cleaning pump 26 is installed below the water storage tank 27, the cleaning pump 26 is connected with the water storage tank 27 through a pipeline, a cleaning pipeline 28 is installed on one side, close to the rotating shaft 24, of the cleaning pump 26, the cleaning pipeline 28 is fixedly connected with the cleaning pump 26, the distilled water can be collected by the aid of the water storage tank 27, the filter basket 19 can be washed by the aid of the cleaning pump 26 matched with the water storage tank, practicability of the device is improved, waste is avoided, and use cost of the device is reduced.
Further, a liquid transfer pipe 12 is installed on one side of the lower end of the liquid separation adjusting washing box 11, a reflux reaction kettle 13 is installed at the lower end of the liquid transfer pipe 12, an evaporation heat exchange pipe 14 is installed outside the reflux reaction kettle 13, the evaporation heat exchange pipe 14 is fixedly connected with the reflux reaction kettle 13 through a clamping groove, a partition plate 15 is installed at the lower end of the reflux reaction kettle 13, a reaction box 16 is installed at the lower end of the partition plate 15, the reaction box 16 is fixedly connected with the partition plate 15, a reaction heat exchange pipe 17 is installed outside the reaction box 16, the reaction heat exchange pipe 17 is fixedly connected with the reaction box 16 through a clamping groove, a material box 4 is installed at the lower end inside the main body support 1, the material box 4 is slidably connected with the main body support 1 through a clamping groove, a filter basket 19 is installed at the upper end inside the material box 4, the filter basket 19 is connected with the material box 4 through a clamping groove, and a discharge pipeline 22 is installed at the lower end of the liquid separation adjusting washing box 11, discharge pipe way 22 and divide liquid to adjust washing tank 11 and the equal fixed connection of main part support 1, firm support 18 is installed to the lower extreme of main part support 1, agitator motor 3 is installed to the upper end of upper portion support 2, agitator motor 3 passes through the coupling joint with pivot 24, filter basket 19 can the rapid filtration insoluble substance in the installation of 4 upper ends of material case, obtain the product rapidly, the staff of being convenient for simultaneously clears away insoluble substance, it is more convenient to make the device use, reduce staff's the work degree of difficulty.
A preparation method of a multi-step integrated device for preparing buprofezin comprises the following steps:
the method comprises the following steps: the method comprises the following steps that a worker adds raw materials and water into a raw material primary treatment box 20, then a stirring motor 3 is powered to drive a rotating shaft 24 to rotate, so that a stirring fan blade 23 is used for stirring materials to fully dissolve the materials, then a material solution is heated through a treatment heat exchange tube 21, a certain amount of hydrochloric acid is dripped, heat is preserved for four hours, the stirring motor 3 is powered off after a period of reaction time, the treatment heat exchange tube 21 is used for cooling the material solution, and the material solution is layered;
step two: the liquid separation cylinder 6 extends to push the push plate 7 to move, so that the liquid absorption elastic hose 9 is in contact with the liquid separation pipe 25, and then the liquid separation pump 8 pumps the liquid after separation into the liquid separation regulation washing box 11;
step three: adding an alkaline aqueous solution into an upper oil layer obtained after liquid separation in a liquid separation regulation washing tank 11, washing, regulating the pH value of a material by washing to 6.8-7.2, then feeding the material into a reflux reaction kettle 13 through a pipette 12, then heating the material through an evaporation heat exchange tube 14, refluxing the material until no water exists to obtain light yellow transparent liquid, collecting the separated water in a water storage tank 27, feeding the material into a reaction tank 16, adding a catalyst into the reaction tank 16 by a worker, increasing the temperature of the material and the catalyst through the reaction heat exchange tube 17, and carrying out heat preservation reaction for six hours;
step four: after a certain period of reaction, the product is discharged into the material box 4, and insoluble substances in the product are filtered out by the filter basket 19.
The working principle is as follows: when the device is used, a worker adds raw materials and water into a raw material primary treatment box 20, then a stirring motor 3 is electrified to drive a rotating shaft 24 to rotate, so that a stirring fan blade 23 stirs materials to fully dissolve the materials, then a material solution is heated through a treatment heat exchange tube 21, a certain amount of hydrochloric acid is dripped, the temperature is kept for four hours, after a period of reaction time, the stirring motor 3 is deenergized, the treatment heat exchange tube 21 cools the material solution to generate a layering phenomenon of the material solution, then a liquid separation cylinder 6 extends to push a push plate 7 to move, so that a liquid absorption elastic hose 9 is contacted with a liquid separation tube 25, then a liquid separation pump 8 pumps the layered liquid into a liquid separation regulation washing box 11, then an alkaline aqueous solution is added into an upper oil layer obtained after liquid separation in the liquid separation regulation washing box 11 for washing, then the material pH value is regulated through water washing to ensure that the pH value is 6.8-7.2, then the mixture enters a reflux reaction kettle 13 through a pipette 12, then a heat exchange tube 14 is evaporated to heat the material, the reflux is carried out until no water exists, a light yellow transparent liquid is obtained, the separated water is collected in a water storage tank 27, the material enters a reaction tank 16, a worker adds a catalyst into the reaction tank 16, the temperature of the material and the catalyst is increased through a reaction heat exchange tube 17, the heat preservation reaction is carried out for six hours, after the reaction is carried out for a period of time, the product is discharged into a material tank 4, a filter basket 19 is used for filtering out insoluble substances in the product, a liquid separating tube 25 is arranged in a rotating shaft 24, the liquid separating treatment can be carried out on the layered liquid in a raw material primary treatment tank 20 under the condition that the rotating shaft 24 drives a stirring fan blade 23 to rotate, the liquid separation is not needed, the liquid separation can be directly carried out, the operation steps are reduced, and the production efficiency is increased, simultaneously stopped the loss of material when carrying out the liquid-transfering, avoid causing the waste, increase the result of use of device, installation imbibition elastic hose 9 makes its cooperation divide liquid cylinder 6 can communicate branch liquid pipe 25, it draws out device inside layering liquid to be convenient for divide liquid pump 8, increase the practicality of device, filter basket 19 can the rapid filtration insoluble substance in the installation of material case 4 upper end, obtain the product rapidly, the staff of being convenient for simultaneously clears away the insoluble substance, it is more convenient to make the device use, reduce staff's the work degree of difficulty, installation water storage tank 27 can collect the distilled water, make its cooperation scavenging pump 26 can wash filter basket 19, increase the practicality of device, avoid causing the waste, the use cost of device is reduced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (8)

1. The utility model provides a buprofezin preparation is with multistage integrated device, includes main part support (1), its characterized in that: upper portion support (2) are installed to the upper end of main part support (1), mounting panel (5) are all installed to the both sides of main part support (1) upper end, the internally mounted of main part support (1) has pivot (24), the inside of pivot (24) is provided with divides liquid pipe (25), the one side that pivot (24) were kept away from in mounting panel (5) is installed and is divided liquid cylinder (6), divide liquid cylinder (6) to be close to one side of pivot (24) and install push pedal (7), the internally mounted of push pedal (7) has imbibition elastic hose (9), the one end that pivot (24) were kept away from in imbibition elastic hose (9) is installed and is divided liquid pump (8), divide liquid pump (8) to keep away from the one end of pivot (24) and install and annotate liquid pipe (10), the externally mounted of pivot (24) has stirring fan blade (23), raw materials preliminary treatment case (20) is installed to the inside upper end of main part support (1), the liquid separation adjusting washing box (11) is installed below the raw material primary treatment box (20), and a treatment heat exchange pipe (21) is installed outside the raw material primary treatment box (20).
2. A multi-step integrated apparatus for buprofezin preparation according to claim 1, characterized in that: the utility model discloses a washing machine, including main part support (1), water storage tank (27) are installed to one side of the inside lower extreme of main part support (1), water storage tank (27) and main part support (1) fixed connection, scavenging pump (26) are installed to the below of water storage tank (27), scavenging pump (26) pass through the pipe connection with water storage tank (27), scavenging pump (26) are close to one side of pivot (24) and install washing pipeline (28), washing pipeline (28) and scavenging pump (26) fixed connection.
3. A multi-step integrated apparatus for buprofezin preparation according to claim 1, characterized in that: liquid separation regulation washing case (11) one side of lower extreme installs pipette (12), backflow reaction cauldron (13) are installed to the lower extreme of pipette (12), backflow reaction cauldron's (13) externally mounted has evaporation heat exchange tube (14), evaporation heat exchange tube (14) pass through draw-in groove fixed connection with backflow reaction cauldron (13).
4. A multi-step integrated apparatus for buprofezin preparation according to claim 3, characterized in that: division board (15) are installed to the lower extreme of backward flow reation kettle (13), division board (15) and backward flow reation kettle (13) fixed connection, reaction box (16) are installed to the lower extreme of division board (15), reaction box (16) and division board (15) fixed connection, reaction heat exchange tube (17) are reacted to the externally mounted of reaction box (16), reaction heat exchange tube (17) pass through draw-in groove fixed connection with reaction box (16).
5. A multi-step integrated apparatus for buprofezin preparation according to claim 1, characterized in that: the material box is characterized in that a material box (4) is installed at the lower end inside the main body support (1), and the material box (4) is connected with the main body support (1) in a sliding mode through a clamping groove.
6. A multi-step integrated apparatus for buprofezin preparation according to claim 5, characterized in that: the filter basket (19) is installed at the upper end of the interior of the material box (4), and the filter basket (19) is connected with the material box (4) through a clamping groove.
7. A multi-step integrated apparatus for buprofezin preparation according to claim 1, characterized in that: divide the liquid to adjust the lower extreme of wash tank (11) and install discharge pipe way (22), discharge pipe way (22) and divide the liquid to adjust wash tank (11) and the equal fixed connection of main part support (1), firm support (18) are installed to the lower extreme of main part support (1), agitator motor (3) are installed to the upper end of upper portion support (2), agitator motor (3) pass through the coupling joint with pivot (24).
8. A method for preparing a multi-step integrated device for preparing buprofezin is realized on the basis of the multi-step integrated device for preparing buprofezin according to any one of claims 1 to 7, and is characterized by comprising the following steps:
the method comprises the following steps: the method comprises the following steps that a worker adds raw materials and water into a raw material primary treatment box (20), then a stirring motor (3) is electrified to drive a rotating shaft (24) to rotate, so that stirring blades (23) stir materials, the materials are fully dissolved, then a material solution is heated through a treatment heat exchange tube (21), a certain amount of hydrochloric acid is dripped, heat preservation is carried out for four hours, after a period of reaction time, the stirring motor (3) is powered off, the treatment heat exchange tube (21) cools the material solution, and the material solution is layered;
step two: the liquid separation air cylinder (6) extends to push the push plate (7) to move, so that the liquid absorption elastic hose (9) is in contact with the liquid separation pipe (25), and then the liquid separation pump (8) pumps the layered liquid into the liquid separation regulation washing box (11);
step three: adding an alkaline aqueous solution into an upper oil layer obtained after liquid separation in a liquid separation regulation washing tank (11), washing, regulating the pH value of a material by washing to be 6.8-7.2, then feeding the material into a reflux reaction kettle (13) through a pipette (12), then heating the material by an evaporation heat exchange tube (14), refluxing the material with water until no water exists to obtain a light yellow transparent liquid, collecting the separated water in a water storage tank (27), feeding the material into a reaction tank (16), adding a catalyst into the reaction tank (16) by a worker, increasing the temperature of the material and the catalyst by the reaction heat exchange tube (17), and carrying out heat preservation reaction for six hours;
step four: after reacting for a period of time, the product is discharged into a material box (4), and insoluble substances in the product are filtered out by a filter basket (19).
CN202110775264.4A 2021-07-08 2021-07-08 Multi-step integrated device for preparing buprofezin and preparation method thereof Pending CN113578218A (en)

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CN202110775264.4A CN113578218A (en) 2021-07-08 2021-07-08 Multi-step integrated device for preparing buprofezin and preparation method thereof

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100234613A1 (en) * 2007-10-25 2010-09-16 Beijing Tianqing Chemicals Co., Ltd process for continuously producing 3-isothiazolinone derivatives and intermediate products thereof
CN103663825A (en) * 2012-09-18 2014-03-26 常州市武进长虹结晶器有限公司 Cleaning system for copper pipes subjected to electroplating
CN208449294U (en) * 2018-03-28 2019-02-01 江苏安邦电化有限公司 A kind of device preparing Buprofezin
CN212383232U (en) * 2020-06-01 2021-01-22 成武县晨晖环保科技有限公司 Liquid-liquid separation device in pinacolone production process
CN112724056A (en) * 2020-12-28 2021-04-30 安道麦安邦(江苏)有限公司 Method and device for effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butylthiourea mother liquor to improve yield

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100234613A1 (en) * 2007-10-25 2010-09-16 Beijing Tianqing Chemicals Co., Ltd process for continuously producing 3-isothiazolinone derivatives and intermediate products thereof
CN103663825A (en) * 2012-09-18 2014-03-26 常州市武进长虹结晶器有限公司 Cleaning system for copper pipes subjected to electroplating
CN208449294U (en) * 2018-03-28 2019-02-01 江苏安邦电化有限公司 A kind of device preparing Buprofezin
CN212383232U (en) * 2020-06-01 2021-01-22 成武县晨晖环保科技有限公司 Liquid-liquid separation device in pinacolone production process
CN112724056A (en) * 2020-12-28 2021-04-30 安道麦安邦(江苏)有限公司 Method and device for effectively utilizing buprofezin intermediate 1-isopropyl-3-tert-butylthiourea mother liquor to improve yield

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