Method and device for recrystallizing anilofos

Abstract

The invention provides an anilofos recrystallization method and device, and relates to the technical field of pesticide production.The anilofos recrystallization device comprises a bearing base, a first support, a bearing support, a second support, a bearing support and a crystallization kettle; an assembly supporting column is fixedly arranged on the top of the bearing base. The first support is fixedly installed on the side face of the bearing base. The bearing bracket is fixedly arranged at the top of the dissolving kettle; the second support is fixedly installed on the side face of the bearing base. The bearing support is fixedly installed at the top end of the assembly supporting column. The crystallization kettle is fixedly mounted at the top of the mounting support; step-by-step cooling is carried out through a crystallization kettle according to a set cooling program, solid anilofos is transferred out from a discharging opening in the bottom of the centrifugal separation device after centrifugation is completed, and filtrate is recycled and transferred into the crystallization kettle to be stirred; the problems of high reaction temperature, high product impurity content, non-uniform product and the like caused by high reaction temperature in anilofos synthesis are solved.

Description

Technical Field

[0001] The invention relates to the technical field of pesticide production, and in particular to a method and a device for recrystallizing safamidis. Background Art

[0002] Anilofos (common name in English) has the chemical name: O, O-dimethyl-S-4-chloro-N-isopropylphenylcarbamoylmethyl dithiophosphate, which is a thiophosphate herbicide. Anilofos is one of the three most commonly used organophosphorus herbicides in my country. It can effectively control annual grass weeds in rice fields. It mainly inhibits the synthesis of glutamine by inhibiting glutamine synthetase, thereby destroying cell division in the biosynthesis of amino acids, an important life process in plants, causing plants to stop growing and eventually die. Anilofos can be absorbed by the roots, coleoptiles and young leaves of plants. It is usually applied after crop sowing and before germination. It can be used in rice fields, and can also be safely applied in cotton, rapeseed, corn, wheat, soybeans, peanuts and cucumber fields. Anilofos is of great significance in agricultural safety production.

[0003] Patent CN102260287A discloses a method for preparing the herbicide silanthion, specifically: adding an appropriate amount of phase transfer catalyst to the condensation reaction, condensation and crystallization are completed in one step, cooling the reaction solution after the reaction is completed, silanthion is directly precipitated and crystallized in water, and the silanthion product is obtained by filtering, washing and drying. The shortcomings of this patent are: the optimized reaction temperature is high, silanthion with a measured content of ≥99.0% decomposes slowly when the temperature is greater than 60°C, the impurity content in the water phase after crystallization is high and it is difficult to remove water, and the uniformity of the obtained product is poor.

[0004] Patents BR7804448 and DE2604225 disclose a method for synthesizing safovinate, specifically: dissolving 2-chloro-N-(4-chlorophenyl)-N-isopropylacetamide in an organic solvent, then adding O,O-dimethyl dithiophosphoric acid and an acid-binding agent to react; or adding methyl sulfide ammonium salt to react. After the reaction is completed, extraction, water washing, and stratification are performed, and the organic solvent is removed from the obtained oil layer to obtain safovinate. Since the reaction requires high temperature reaction and high temperature desolventization, both of which will cause safovinate to decompose, the impurity content in the product increases, and the product is not uniform.

[0005] At present, due to the high reaction temperature in the synthesis of safron, there are many disadvantages, such as high reaction temperature, high product impurities, and uneven products. In order to solve this problem, a technology for refining safron is proposed. This technology: low-temperature crystallization, solvent recycling, and the use of a new crystallization device can ensure high product content, uniform quality, high yield, and very little waste, which is friendly to the ecological environment. Summary of the invention

[0006] In view of this, the present invention provides a method and device for recrystallizing safron, which comprises a bearing base, a first support, a load-bearing bracket, a second support, a bearing support and a crystallization kettle, so as to solve the problems of high reaction temperature, high product impurities, and uneven product caused by high reaction temperature in the synthesis of safron.

[0007] The present invention provides a method and device for recrystallizing safflower, which specifically comprises: a bearing base, a first support, a load-bearing bracket, a second support, a bearing support and a crystallization kettle; An assembly pillar is fixedly arranged on the top of the bearing base, a centrifugal separation device is fixedly arranged on the side of the assembly pillar, and a conveying pipe is fixedly arranged on the top of the centrifugal separation device; a first support is fixedly installed on the side of the bearing base, a bearing bracket is fixedly installed on the top of the first support, a dissolving kettle is fixedly installed on the top of the bearing bracket, a conveying side pump is arranged on the side of the dissolving kettle, a material transfer pipe is arranged at the bottom of the dissolving kettle, a recovery pipe is arranged on the top of the dissolving kettle, and a first valve is fixedly arranged on one end of the recovery pipe; a load-bearing bracket is fixedly arranged on the top of the dissolving kettle; a second support is fixedly installed on the side of the bearing base, and a An assembly bracket is provided, a melting carrier cylinder and a recovery side cylinder are fixedly arranged on the top of the assembly bracket, and a material transfer side pump is arranged on the side of the melting carrier cylinder; a bearing support is fixedly installed on the top of the assembly pillar, a control device is fixedly installed on the top of the bearing support, an assembly carrier is fixedly installed on the top of the bearing support, and a mounting support is fixedly installed on the top of the assembly carrier; a crystallization kettle is fixedly installed on the top of the mounting support, a bearing shaft is rotatably arranged on the inner side of the crystallization kettle, a scraping blade is fixedly arranged on the outer side of the bearing shaft, a discharge side pump is arranged on the side of the bearing shaft, a cleaning motor is fixedly arranged on the top of the crystallization kettle, and an adding pipe is arranged on the top of the crystallization kettle.

[0008] In at least some embodiments, the centrifugal separation device is further provided with: a conveying connecting pipe and a bearing bottom cylinder on the outside; The conveying connecting pipe is fixedly arranged on the top of the centrifugal separation device; and the bearing bottom cylinder is fixedly arranged on the bottom of the conveying connecting pipe.

[0009] In at least some embodiments, the side of the dissolving kettle is further provided with: a rotating support shaft, a stirring blade and a stirring motor; The rotating support shaft is rotatably arranged inside the dissolving kettle; the stirring blade is fixedly arranged outside the rotating support shaft; and the stirring motor is fixedly installed on the top of the dissolving kettle.

[0010] In at least some embodiments, the top of the load-bearing support is further provided with: a load-bearing support tube and an additional branch pipe; The bearing support tube is fixedly installed on the top of the load-bearing bracket; the additional branch pipe is fixedly arranged on the bottom of the bearing support tube.

[0011] In at least some embodiments, the side of the recovery side cylinder is further provided with: a delivery side pipe and a second valve; The delivery side pipe is fixedly arranged on the side of the recovery side cylinder; and the second valve is fixedly arranged on the side of the delivery side pipe.

[0012] In at least some embodiments, the top of the mounting support is further provided with: a heat-insulating casing frame and a heating support; The heat preservation sleeve frame is fixedly installed on the top of the installation support; the heating support column is fixedly installed on the inner side of the heat preservation sleeve frame.

[0013] In at least some embodiments, the inner side of the crystallization kettle is further provided with: a mounting support ring and a filter screen frame; The mounting support ring is fixedly installed on the inner side of the crystallization kettle; the filter screen frame is arranged on the top of the mounting support ring.

[0014] The method and device for recrystallizing safflower provided by the present invention have the following beneficial effects: The invention provides a bearing base, a first support, a load-bearing bracket, a second support, a bearing support and a crystallization kettle, and performs recrystallization through a crystallization device to obtain a high-content cypermethrin technical. The core technology of the invention is to complete crystallization by using a novel crystallization device. After crystallization, the centrifuged filtrate can continue to serve as a solvent for configuring the cypermethrin mother liquor, and after a certain batch of applications, it is transferred to a distillation recovery device for solvent recovery. The method is energy-saving and efficient, obtains a high-content cypermethrin technical, is environmentally friendly, and has little waste. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solution of the embodiment of the present invention, the drawings of the embodiment are briefly introduced below.

[0016] The drawings described below are only related to some embodiments of the present invention, but are not intended to limit the present invention.

[0017] In the attached picture: Figure 1 It shows a schematic structural diagram of the overall assembly of components of a recrystallization device according to an embodiment of the present invention; Figure 2 It shows a schematic structural diagram of the assembly and disassembly of the whole parts of the bearing base according to an embodiment of the present invention; Figure 3 It shows a schematic structural diagram of the assembly and disassembly of the first support integral component according to an embodiment of the present invention; Figure 4 It shows a schematic structural diagram of the assembly and disassembly of the integral components of the load-bearing bracket according to an embodiment of the present invention; Figure 5 It shows a schematic structural diagram of the assembly and disassembly of the second support integral component according to an embodiment of the present invention; Figure 6 It shows a schematic structural diagram of the assembly and disassembly of the whole components of the bearing support according to an embodiment of the present invention; Figure 7 A schematic structural diagram of the assembly and disassembly of the overall components of a crystallization kettle according to an embodiment of the present invention is shown.

[0018] Reference numerals list 1. Load-bearing base; 101, assembly support; 102, centrifugal separation device; 103, delivery pipe; 104, recovery side pump; 105, bearing bottom cylinder; 2. The first support; 201, bearing support; 202, dissolving kettle; 203, conveying side pump; 204, material transfer pipe; 205, recovery pipe; 206, rotating support shaft; 207, stirring blade; 208, stirring motor; 209, first valve; 3. Load-bearing bracket; 301, bearing support tube; 302, adding branch pipe; 4. The second support; 401, assembly bracket; 402, melting carrier cylinder; 403, transfer side pump; 404, recovery side cylinder; 405, delivery side pipe; 406, second valve; 5. Bearing support; 501, control device; 502, assembly carrier; 503, mounting support; 504, insulation frame; 505, heating support; 6. Crystallization kettle; 601. Bearing shaft; 602. Scraping blades; 603. Discharge side pump; 604. Cleaning motor; 605. Installing support ring; 606. Filter frame; 607. Adding connecting pipe. DETAILED DESCRIPTION

[0019] The following describes in detail various embodiments of the present invention in conjunction with the accompanying drawings; Example: Please refer to Figures 1 to 7 : The present invention proposes a method and device for recrystallizing safflower, comprising: a bearing base 1, a first support 2, a load-bearing bracket 3, a second support 4, a bearing support 5 and a crystallization kettle 6; An assembly pillar 101 is fixedly provided on the top of the bearing base 1, a centrifugal separation device 102 is fixedly installed on the side of the assembly pillar 101, and a conveying pipe 103 is fixedly provided on the top of the centrifugal separation device 102; the first support 2 is fixedly installed on the side of the bearing base 1, a bearing bracket 201 is fixedly installed on the top of the first support 2, a dissolving kettle 202 is fixedly installed on the top of the bearing bracket 201, a conveying side pump 203 is provided on the side of the dissolving kettle 202, a material transfer pipe 204 is provided at the bottom of the dissolving kettle 202, a recovery pipe 205 is provided on the top of the dissolving kettle 202, and a first valve 209 is fixedly provided at one end of the recovery pipe 205; the load-bearing support 3 is fixedly provided on the top of the dissolving kettle 202; the second support 4 is fixedly installed on the side of the bearing base 1, and a An assembly bracket 401 is provided, on the top of which a melting carrier cylinder 402 and a recovery side cylinder 404 are fixedly arranged, and on the side of which a material transfer side pump 403 is arranged; a bearing support 5 is fixedly installed on the top of the assembly pillar 101, on the top of which a control device 501 is fixedly installed, on the top of which an assembly carrier 502 is fixedly installed, and on the top of which a mounting support 503 is fixedly installed; a crystallization kettle 6 is fixedly installed on the top of the mounting support 503, on the inner side of the crystallization kettle 6 a bearing shaft 601 is rotatably arranged, on the outer side of the bearing shaft 601 a scraping blade 602 is fixedly arranged, on the side of the bearing shaft 601 a discharge side pump 603 is arranged, on the top of the crystallization kettle 6 a cleaning motor 604 is fixedly arranged, and on the top of the crystallization kettle 6 an adding pipe 607 is arranged.

[0020] Embodiment 1: Figures 3 to 7 As shown, the side of the recovery side tube 404 is also provided with: a delivery side pipe 405 and a second valve 406; the delivery side pipe 405 is fixedly arranged on the side of the recovery side tube 404; the second valve 406 is fixedly arranged on the side of the delivery side pipe 405; the top of the mounting support 503 is also provided with: an insulation sleeve frame 504 and a heating support 505; the insulation sleeve frame 504 is fixedly installed on the top of the mounting support 503; the heating support 505 is fixedly installed on the inner side of the insulation sleeve frame 504; the inner side of the crystallization kettle 6 is also provided with: an installation support ring 605 and a filter screen frame 606; the installation support ring 605 is fixedly installed on the inner side of the crystallization kettle 6; the filter screen frame 606 is arranged on the top of the installation support ring 605.

[0021] Embodiment 2: Based on Embodiment 1, Figures 2 to 6As shown, the outside of the centrifugal separation device 102 is also provided with: a conveying pipe 103 and a bearing bottom cylinder 105; the conveying pipe 103 is fixedly arranged on the top of the centrifugal separation device 102; the bearing bottom cylinder 105 is fixedly arranged at the bottom of the conveying pipe 103; the side of the dissolving kettle 202 is also provided with: a rotating support shaft 206, a stirring blade 207 and a stirring motor 208; the rotating support shaft 206 is rotatably arranged on the inside of the dissolving kettle 202; the stirring blade 207 is fixedly arranged on the outside of the rotating support shaft 206; the stirring motor 208 is fixedly installed on the top of the dissolving kettle 202; the top of the load-bearing bracket 3 is also provided with: a bearing support cylinder 301 and an addition branch pipe 302; the bearing support cylinder 301 is fixedly installed on the top of the load-bearing bracket 3; the addition branch pipe 302 is fixedly arranged at the bottom of the bearing support cylinder 301.

[0022] Specific usage and function of this embodiment: In the present invention, the molten sulphuric acid and acetonitrile are transferred to the dissolving kettle 202. After being stirred evenly, the crystallization mother liquor is kept at 40° C. for 30 minutes in the dissolving kettle 202. After the heat preservation is completed, the sulphuric acid crystallization mother liquor is transferred to the crystallization kettle 6 through the delivery side pump 203; The crystallization kettle 6 is cooled step by step according to the set cooling program through the heating support 505, and maintained at 20°C for 1 hour and then maintained at 0°C for 1 hour. After the crystallization is completed, the material is transferred to the centrifugal separation device 102 through the discharge port at the bottom for centrifugation. After the centrifugation is completed, the solid silanol is transferred to the supporting bottom cylinder 105 at the discharge port at the bottom of the centrifugal separation device 102, and the filtrate is transferred to the crystallization kettle 6 through the recovery side pump 104.

Claims

1. A device for recrystallizing safflower, comprising: A bearing base (1), a first support (2), a load-bearing bracket (3), a second support (4), a bearing support (5) and a crystallization kettle (6); The top of the bearing base (1) is fixedly provided with an assembly pillar (101), a centrifugal separation device (102) is fixedly installed on the side of the assembly pillar (101), and a conveying pipe (103) is fixedly installed on the top of the centrifugal separation device (102); the first support (2) is fixedly installed on the side of the bearing base (1), a bearing bracket (201) is fixedly installed on the top of the first support (2), a dissolving kettle (202) is fixedly installed on the top of the bearing bracket (201), a conveying side pump (203) is arranged on the side of the dissolving kettle (202), a material transfer pipe (204) is arranged at the bottom of the dissolving kettle (202), a recovery pipe (205) is arranged on the top of the dissolving kettle (202), and a first valve (209) is fixedly installed at one end of the recovery pipe (205); the load-bearing bracket (3) is fixedly installed on the top of the dissolving kettle (202); the second support (4) is fixedly installed on the side of the bearing base (1), and the top of the second support (4) is fixedly installed An assembly bracket (401) is fixedly arranged, a melting carrier tube (402) and a recovery side tube (404) are fixedly arranged on the top of the assembly bracket (401), and a material transfer side pump (403) is arranged on the side of the melting carrier tube (402); the bearing support (5) is fixedly installed on the top of the assembly pillar (101), a control device (501) is fixedly installed on the top of the bearing support (5), an assembly carrier (502) is fixedly installed on the top of the bearing support (5), and a mounting support (503) is fixedly installed on the top of the assembly carrier (502); the crystallization kettle (6) is fixedly installed on the top of the mounting support (503), a bearing shaft (601) is rotatably arranged inside the crystallization kettle (6), a scraping blade (602) is fixedly arranged outside the bearing shaft (601), a discharge side pump (603) is arranged on the side of the bearing shaft (601), a cleaning motor (604) is fixedly arranged on the top of the crystallization kettle (6), and an adding pipe (607) is arranged on the top of the crystallization kettle (6).

2. The device for recrystallizing thiamethoxam according to claim 1, characterized in that: The centrifugal separation device (102) is further provided with a conveying connecting pipe (103) and a bearing bottom cylinder (105) on the outside; The conveying connecting pipe (103) is fixedly arranged on the top of the centrifugal separation device (102); and the supporting bottom cylinder (105) is fixedly arranged on the bottom of the conveying connecting pipe (103).

3. The device for recrystallization of safflower according to claim 1, characterized in that: The side of the dissolving kettle (202) is also provided with: a rotating support shaft (206), a stirring blade (207) and a stirring motor (208); The rotating support shaft (206) is rotatably disposed inside the dissolving kettle (202); the stirring blade (207) is fixedly disposed outside the rotating support shaft (206); and the stirring motor (208) is fixedly installed on the top of the dissolving kettle (202).

4. The device for recrystallizing thiamethoxam according to claim 1, characterized in that: The top of the load-bearing support (3) is also provided with: a load-bearing support tube (301) and an additional branch pipe (302); The bearing support tube (301) is fixedly mounted on the top of the load-bearing bracket (3); and the additional branch pipe (302) is fixedly arranged on the bottom of the bearing support tube (301).

5. The device for recrystallization of safflower according to claim 1, characterized in that: The side surface of the recovery side cylinder (404) is also provided with: a delivery side pipe (405) and a second valve (406); The delivery side pipe (405) is fixedly arranged on the side of the recovery side tube (404); and the second valve (406) is fixedly arranged on the side of the delivery side pipe (405).

6. The device for recrystallization of safflower according to claim 1, characterized in that: The top of the mounting support (503) is also provided with: a heat-insulating casing frame (504) and a heating support pillar (505); The heat-insulating casing frame (504) is fixedly mounted on the top of the mounting support (503); and the heating support pillar (505) is fixedly mounted on the inner side of the heat-insulating casing frame (504).

7. The device for recrystallizing safamidis according to claim 1, characterized in that: The inner side of the crystallization kettle (6) is also provided with: a mounting support ring (605) and a filter screen frame (606); The mounting support ring (605) is fixedly mounted on the inner side of the crystallization kettle (6); and the filter screen frame (606) is arranged on the top of the mounting support ring (605).

8. A method for using the device for recrystallization of saffos according to any one of claims 1 to 7, characterized in that: The following steps are involved: First, the molten liquid of safovate and the crystallization solvent are respectively transferred into a dissolving kettle (202) to prepare a safovate crystallization mother liquor. After the crystallization mother liquor is stirred evenly, it is kept warm in the dissolving kettle (202) for a period of time. After the heat preservation is completed, the safovate crystallization mother liquor is transferred into a crystallization kettle (6); Afterwards: the crystallization kettle (6) is cooled step by step according to the set cooling program. After the crystallization is completed, the material is transferred to the centrifugal separation device (102) through the discharge port at the bottom of the crystallization kettle (6) for centrifugation. After the centrifugation is completed, the solid safflower is transferred to the supporting bottom cylinder (105) through the discharge port at the bottom of the centrifugal separation device (102), and the filtrate is transferred to the crystallization kettle (6).

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