A crystallization apparatus for indaziflam

Abstract

The application provides a crystallization device for indaziflam, which comprises a crystallization kettle and a distillation tank. The crystallization kettle is internally provided with a cooling circulation device and a stirring system, and the bottom of the crystallization kettle is connected with the distillation tank through a first filtrate pipe. The distillation tank is internally provided with an inner container and a heat circulation device, solid-liquid separation is realized through a second filtrate pipe, and the distillation mother liquor is circulated back to the crystallization kettle through a pipeline. The structure realizes secondary distillation treatment of the mother liquor, effectively recovers unreacted raw materials and organic solvents, significantly improves the utilization rate of raw materials, reduces the production cost, and reduces the emission of pollutants. The device realizes the synergistic effect of the heat circulation and the cooling system, realizes efficient energy utilization, and forms a green and sustainable crystallization process.

Description

Technical Field

[0001] This utility model relates to the technical field of pesticide crystallization equipment, specifically to a crystallization device for indazine-flufenoxam. Background Technology

[0002] With the development of pesticide synthesis technology, crystallization is a crucial step in the production of indazedifluazine, an important pesticide intermediate, as its effectiveness directly impacts product purity, yield, and the ease of subsequent processing. Indazedifluazine typically crystallizes in solvents such as alcohols, alcohol-water mixtures, and amides. Lowering the solution temperature reduces the solubility of indazedifluazine, causing crystals to precipitate—this is one of the most common crystallization methods. However, existing indazedifluazine crystallization devices often employ simple filtration systems, using only single or double-layer filters. This is insufficient to effectively remove minute impurities and particles from the mother liquor, affecting product purity and hindering the full recovery and utilization of residual solvents and active ingredients. Direct discharge of the mother liquor not only increases raw material consumption but may also lead to environmental pollution. Summary of the Invention

[0003] This invention provides an indazine-flutamide crystallization device to solve the problems of raw material consumption and environmental pollution caused by the direct discharge of mother liquor in indazine-flutamide crystallization devices.

[0004] To address the aforementioned problems, this utility model provides an indazine-flutamide crystallization device, comprising: a crystallization vessel; a cooling circulation device fixedly disposed on the side wall of the crystallization vessel; a first filtrate pipe disposed at the outlet of the crystallization vessel and communicating with the inner layer of the crystallization vessel; a flow control valve disposed above the first filtrate pipe; several layers of filter screens disposed below the flow control valve; a crystallization outlet disposed on one side of the filter screens; a distillation tank connected to the first filtrate pipe via a first connecting pipe; a first water pump device disposed in the middle section of the first connecting pipe; and a heat circulation device fixedly disposed on the side wall of the distillation tank. Through this solution, the addition of a distillation tank allows for secondary distillation of the mother liquor directly discharged in the traditional process, effectively recovering unreacted raw materials and organic solvents, avoiding the waste of raw materials caused by direct discharge of mother liquor in the traditional method, improving the overall utilization rate of indazine-flutamide, and reducing production costs.

[0005] According to one embodiment of the present invention, the crystallization vessel further includes: a liquid inlet located at the top of the crystallization vessel, a catalyst inlet located at the top of the crystallization vessel, a stirring motor located at the center of the top of the crystallization vessel, a stirring device connected to the stirring motor and located at the bottom of the inner layer, a first filter pipe located at the bottom of the crystallization vessel and connected to the bottom of the inner layer, and a crystallization outlet located in the middle of the first filter pipe. Through the above scheme, the overall design structure of the crystallization vessel is compact and the layout of each component is reasonable, making operation simpler and maintenance easier.

[0006] According to one embodiment of the present invention, the distillation tank further includes: a mother liquor inlet connected to the distillation tank via a first connecting pipe; an inner liner disposed within the distillation tank; a second filter pipe disposed at the bottom of the distillation tank and connected to the inner liner; a solid waste outlet located in the middle of the second filter pipe and connected to the filter screen disposed within the second filter pipe; a circulating boiling hot liquid outlet disposed at the top of the heat circulation device and connected to the outer layer of the distillation tank via a pipe; and a circulating boiling hot liquid inlet disposed on the side wall of the heat circulation device and connected to the distillation tank via a pipe. Through the above scheme, it is ensured that the mother liquor discharged from the crystallization vessel can smoothly enter the distillation tank for secondary treatment, improving the purity of the mother liquor, enabling further recycling of the mother liquor, and reducing the waste of raw materials.

[0007] According to one embodiment of the present invention, the outlet of the distillation tank is connected to the inlet of the mother liquor of the crystallization vessel through a second connecting pipe. A second water pump device is provided in the middle section of the second connecting pipe. By recycling the mother liquor, the demand for fresh raw materials is reduced, thereby optimizing resource allocation and reducing production costs.

[0008] According to one embodiment of the present invention, the filter layer includes a coarse filter layer, a fine filter layer and an activated carbon adsorption layer arranged sequentially. The coarse filter layer is made of stainless steel mesh material, and the fine filter layer uses high-precision polytetrafluoroethylene membrane filter material. The stainless steel coarse filter layer (80-100 mesh) pre-treats suspended impurities, and the polytetrafluoroethylene fine filter layer (0.2μm pore size) intercepts submicron particles, forming a dual barrier of "mechanical screening-membrane retention", which further reduces the consumption of raw materials.

[0009] According to one embodiment of this utility model, the filter layer is connected by a threaded connection or a quick snap connection. The use of threaded connection or quick snap connection makes the installation and disassembly of the filter layer simple and quick. When the filter layer becomes clogged or damaged due to long-term use, the staff can quickly replace or clean it, thereby reducing downtime and improving the operating efficiency of the equipment.

[0010] According to one embodiment of the present invention, both the inner layer and the inner wall of the inner liner are provided with a polytetrafluoroethylene composite anti-scaling coating. By coating the inner layer and the inner wall of the inner liner with a PTFE composite coating, the risk of scaling of indazine fluroxypyr and its mother liquor during crystallization and distillation is significantly reduced, thus maintaining the cleanliness and efficient operation of the equipment.

[0011] According to one embodiment of the present invention, the feed inlet of the first filter tube is connected to the crystallization outlet through a transparent pipe. The transparent pipe allows the staff to directly observe the state of the liquid flowing out of the crystallization outlet, thereby timely judging the progress and effect of the crystallization process, promptly identifying and solving potential problems, and ensuring the stability of the production process and product quality.

[0012] According to one embodiment of the present invention, the crystallizing vessel is provided with a first exhaust valve at the top of its outer layer, and the distillation tank is provided with a second exhaust valve on its outer layer. The exhaust valves are provided to release the gas generated in the crystallizing vessel and the distillation tank during operation in a timely manner, so as to avoid excessive internal pressure that could lead to equipment damage or safety accidents.

[0013] According to one embodiment of the present invention, the cooling circulation device is equipped with a plate heat exchanger and a transfer pump. The heat circulation device is equipped with a heat exchanger and a transfer pump. The heat exchanger is equipped with a temperature sensor. The plate heat exchanger can provide high heat exchange efficiency and quickly transfer heat from the material in the crystallization vessel to the cooling medium to achieve a rapid cooling effect.

[0014] The technical advantages of this application are as follows: This application provides an indazine-flufenoxam crystallization apparatus that treats the mother liquor in a distillation tank and then returns the distilled mother liquor to the crystallization kettle, reducing resource waste, lowering production costs, and minimizing environmental pollution. Simultaneously, the use of a three-layer filter effectively separates the crystals and the mother liquor, improving product purity. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the overall structure of an indazine-fluoxam crystallization device provided by this utility model.

[0016] Figure 2 This is a top view structural diagram of an indazine-fluoxam crystallization device provided by this utility model.

[0017] Figure 3 This utility model provides Figure 2 A schematic diagram of section AA.

[0018] Figure 4 This utility model provides Figure 3 A magnified view of the details at point B in the middle.

[0019] Explanation of reference numerals in the attached figures: 1. Crystallization vessel; 101. Stirring motor; 102. Liquid inlet; 103. Inner layer; 104. Stirring device; 105. Distillation mother liquor inlet; 106. First triangular prism support; 107. Stirring blades; 108. Filter screen layer; 109. First filtrate pipe; 110. Crystallization outlet; 111. Flow control valve; 112. First exhaust valve; 113. Catalyst inlet; 2. Cooling circulation device; 3. First water pump unit; 301. First connecting pipe; 4. Distillation tank; 401. Mother liquor inlet; 402. Second vent valve; 403. Inner liner; 404. Second filter tube; 405. Solid waste outlet; 406. Second triangular prism support; 5. Heat circulation device; 501. Circulating boiling hot liquid outlet; 502. Circulating boiling hot liquid inlet; 6. Second water pump device; 601. Second connecting pipe. Detailed Implementation

[0020] The following will be combined with the appendix Figures 1-4 The embodiments of the technical solution of this application are described in detail below. The following embodiments are only used to illustrate the technical solution of this application more clearly, and are therefore only examples and should not be used to limit the scope of protection of this application.

[0021] Example 1 Reference Figure 1 and Figure 2 This invention provides a crystallization device for indazine-flufenoxam, comprising a crystallization vessel 1 with a support frame fixed at its bottom to ensure stability. The crystallization vessel 1 has an inner layer 103, forming a space between the inner layer 103 and the crystallization vessel 1, which can be used for circulating cooling liquid. The top of the crystallization vessel 1 is provided with a liquid inlet 102, a catalyst inlet 113, and a stirring motor 101. The stirring motor 101 is connected to a stirring device 104, and the rotating shaft of the stirring device 104 is provided with stirring blades 107, which are located at the bottom of the inner layer 103, for mixing materials to ensure sufficient crystallization of indazine-flufenoxam and prevent crystallization on the wall of the inner layer 103. A first filtrate pipe 109 is provided at the bottom, communicating with the bottom of the inner layer 103 for discharging filtrate.

[0022] The first filtrate pipe 109 is equipped with a flow control valve 111 and a three-layer filter screen 108, including a coarse filter layer, a fine filter layer, and an activated carbon adsorption layer arranged sequentially. The coarse filter layer is made of stainless steel mesh, and the fine filter layer uses high-precision polytetrafluoroethylene membrane filter material. The three-layer filter screen 108 are connected by threaded connections or quick-clamp connections for easy replacement and cleaning. The crystallization outlet 110 is located on the downward-sloping side of the filter screen layer 108. A first exhaust valve 112 is provided at the top of the outer layer for discharging gas from the jacket. The cooling circulation device 2 is located on the first triangular prism support 106 and connected to the outer layer of the crystallization vessel 1. It is equipped with a plate heat exchanger and a transfer pump for cooling the crystallization vessel 1.

[0023] The crystallization apparatus also includes a distillation tank 4, with a support frame fixed to its bottom. The distillation tank 4 has an inner liner 403, forming a space between the inner liner 403 and the distillation tank 4, which is used for the circulation of the boiling hot circulating liquid medium. A second filter pipe 404 is located at the bottom of the inner liner 403, and a solid waste outlet 405 is located on the second filter pipe 404. A mother liquor inlet 401 is located at the top, connected to the first filter pipe 109 of the crystallization vessel 1 via a first connecting pipe 301. The distillation tank 4 is also connected to the distillation mother liquor inlet 105 at the top of the crystallization vessel 1 via a second connecting pipe 601, enabling mother liquor circulation. A sampling port is located at the distillation mother liquor inlet 105, allowing for periodic sampling and analysis of the circulating mother liquor and replacement with fresh solvent. A second exhaust valve 402 is located on the outer layer of the distillation tank 4 to discharge gas from the space between the inner and outer liner.

[0024] The heat circulation device 5 is located above the second triangular prism support 406 and is connected to the outer layer of the distillation tank 4 via a pipe. It has a circulating boiling hot liquid outlet 501 at the top and a circulating boiling hot liquid inlet 502 on the side wall. The heat circulation device 5 includes a heat exchanger and a transfer pump. The heat exchanger is equipped with a temperature sensor for heating and temperature control of the distillation tank 4.

[0025] Both the inner layer 103 and the inner liner 403 are coated with a polytetrafluoroethylene composite anti-scaling coating, which significantly reduces the risk of scaling of indazine fluroxypyr and its mother liquor during crystallization and distillation, keeping the equipment clean and operating efficiently.

[0026] The feed inlet of the first filtrate tube 109 is connected to the crystallization outlet 110 by a transparent pipe, which facilitates observation of the filtrate.

[0027] The first connecting pipe 301 is equipped with a first water pump device 3 in the middle section, and the second connecting pipe 601 is equipped with a second water pump device 6 in the middle section, which are used to provide power for the circulation of mother liquor.

[0028] Working principle: Crystallization process: Indomethacin-flufenican material is added to the inner layer 103 of crystallization vessel 1 through inlet 102, and an appropriate amount of catalyst, such as ethanol solution, is added through catalyst inlet 113. Stirring motor 101 is started, driving stirring device 104 to stir the material, ensuring thorough mixing. Cooling circulation device 2 is started, and coolant is delivered to the jacket of crystallization vessel 1 through a plate heat exchanger and a transfer pump to cool crystallization vessel 1, control the crystallization temperature, and promote the crystallization of indomethacin-flufenican. After crystallization, flow control valve 111 is opened, and the filtrate containing crystals flows through the first filtrate pipe 109. Passing through filter screen layer 108, the coarse filter layer, fine filter layer, and activated carbon adsorption layer sequentially filter the filtrate, and the crystals are discharged and collected from crystallization outlet 110.

[0029] Mother liquor treatment process: The filtered mother liquor is transported to the inner liner 403 of the distillation tank 4 via the first connecting pipe 301 and the first water pump device 3. The heat circulation device 5 is activated, and the heat exchanger and the transfer pump circulate the hot boiling liquid between the jacket of the distillation tank 4 and the heat circulation device 5. The temperature sensor of the heat exchanger precisely controls the distillation temperature to distill the mother liquor. Solid waste generated during the distillation process is discharged through the solid waste outlet 405. The distilled mother liquor is transported back to the distillation mother liquor inlet 105 at the top of the crystallization vessel 1 via the second connecting pipe 601 and the second water pump device 6, realizing the recycling of the mother liquor.

[0030] Exhaust operation: During crystallization and distillation, the first exhaust valve 112 and the second exhaust valve 402 are opened respectively to exhaust the generated gas and ensure the safe operation of the device.

[0031] The above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. A crystallization apparatus for indazine-flumethrin, characterized in that, include: Crystallization vessel (1), cooling circulation device (2) fixedly installed on the side wall of the crystallization vessel (1), first filtrate pipe (109) installed at the outlet of the crystallization vessel (1) and connected to the inner layer (103) of the crystallization vessel (1), flow control valve (111) installed above the first filtrate pipe (109), several layers of filter screen (108) installed below the flow control valve (111), crystallization outlet (110) installed on one side of the filter screen (108), distillation tank (4) connected to the first filtrate pipe (109) through a first connecting pipe (301), first water pump device (3) installed in the middle section of the first connecting pipe (301), and heat circulation device (5) fixedly installed on the side wall of the distillation tank (4).

2. The indazine-flumethrin crystallization apparatus according to claim 1, characterized in that, The crystallization vessel (1) further includes: a liquid inlet (102) located at the top of the crystallization vessel (1), a catalyst inlet (113) located at the top of the crystallization vessel (1), a stirring motor (101) located at the center of the top of the crystallization vessel (1), a stirring device (104) connected to the stirring motor (101) and located at the bottom of the inner layer (103), a first filter pipe (109) located at the bottom of the crystallization vessel (1) and connected to the bottom of the inner layer (103), and a crystallization outlet (110) opened in the middle of the first filter pipe (109).

3. The indazine-flumethrin crystallization apparatus according to claim 1, characterized in that, The distillation tank (4) further includes: a mother liquor inlet (401) connected to the distillation tank (4) via the first connecting pipe (301); an inner liner (403) located inside the distillation tank (4); a second filter pipe (404) located at the bottom of the distillation tank (4) and connected to the inner liner (403); a solid waste outlet (405) located in the middle of the second filter pipe (404) and connected to the filter screen located inside the second filter pipe (404); a circulating boiling hot liquid outlet (501) located at the top of the heat circulation device (5) and connected to the outer layer of the distillation tank (4) via a pipe; and a circulating boiling hot liquid inlet (502) located on the side wall of the heat circulation device (5) and connected to the distillation tank (4) via a pipe.

4. The indazine-flumethrin crystallization apparatus according to claim 3, characterized in that, The outlet of the distillation tank (4) is connected to the mother liquor inlet (105) of the crystallization vessel (1) via a second connecting pipe (601), and a second water pump device (6) is provided in the middle section of the second connecting pipe (601).

5. The indazine-flumethrin crystallization apparatus according to claim 1, characterized in that, The filter layer (108) includes a coarse filter layer, a fine filter layer and an activated carbon adsorption layer arranged in sequence. The coarse filter layer is made of stainless steel mesh material and the fine filter layer is made of polytetrafluoroethylene membrane filter material.

6. The indazine-flumethrin crystallization apparatus according to claim 5, characterized in that, The three filter layers (108) are connected by threaded connection or quick snap connection.

7. The indazine-flumethrin crystallization apparatus according to claim 3, characterized in that, Both the inner layer (103) and the inner wall of the inner liner (403) are provided with a polytetrafluoroethylene anti-scaling coating.

8. The indazine-flumethrin crystallization apparatus according to claim 1, characterized in that, The inlet of the first filtrate tube (109) is connected to the crystallization outlet (110) via a transparent pipe.

9. The indazine-flumethrin crystallization apparatus according to claim 1, characterized in that, The crystallization vessel (1) is provided with a first exhaust valve (112) at the top of its outer layer, and the distillation tank (4) is provided with a second exhaust valve (402) at the top of its outer layer.

10. The indazine-flumethrin crystallization apparatus according to claim 1, characterized in that, The cooling circulation device (2) is equipped with a plate heat exchanger and a delivery pump, and the heat circulation device (5) is equipped with a heat exchanger and a delivery pump. The heat exchanger is equipped with a temperature sensor.

Images