A propiconazole distillation method and device

Abstract

The present invention relates to the field of propiconazole production, and in particular to a propiconazole distillation method and device, wherein the distillation device includes a mixing tank, a filtering tank, a separation mechanism, a first distillation mechanism, and a second distillation mechanism, and the separation mechanism can quickly separate the organic phase and the inorganic phase mixed in the mixing tank, and sequentially distill the organic phase through the first distillation mechanism and the second distillation mechanism to obtain an organic solvent and a fine propiconazole product, respectively. Through the above-mentioned device and method, the continuous production of propiconazole is realized, and the influence of the standing and other links in the traditional process on the production efficiency is avoided; the production cost is reduced by the recycling of organic solvents and water; the concentration of propiconazole is accurately controlled by distillation, thereby improving the purity and quality of the propiconazole product.

Description

Technical Field

[0001] The invention relates to the field of propiconazole production, and in particular to a propiconazole distillation method and device. Background Art

[0002] Propiconazole is a systemic triazole fungicide with protective and therapeutic effects. It can be absorbed by roots, stems and leaves and quickly conducted upward in the plant body. It is used to prevent and control diseases caused by ascomycetes, basidiomycetes and deuteromycetes, especially rice blast, rice false smut, sheath blight, seedling blight, wheat take-all, powdery mildew, rust, root rot, banana leaf spot, etc. It has a good preventive effect.

[0003] There are generally three methods for the synthesis of propiconazole, namely bromination, chlorination and post-cyclization. Currently, the most widely used synthesis process is to use 2,4-dichloroacetophenone as the raw material, first bromination, then cyclization with 1,2-pentanediol, and finally condensation with 1,2,4-triazole sodium to produce propiconazole.

[0004] When using the above synthesis process to prepare propiconazole, in order to ensure the purity of the propiconazole product, the synthesized product needs to be further purified. An organic solvent is added to the crude propiconazole, and after washing with water, it is allowed to stand, and the upper organic phase is taken for distillation. The propiconazole in the middle section of the distillation is taken as a product with higher purity. After the first section and the tail section products are cyclically distilled, a portion of high-purity propiconazole products are obtained.

[0005] The above-mentioned process requires a standing process, which slows down the production rhythm, wastes a lot of production time, and leads to low efficiency of product production; in addition, during the distillation process, the critical points of the front section, middle section, and back section cannot be clearly distinguished, resulting in the inability to timely recover some propiconazole products, or affecting the purity of the recovered propiconazole products. Summary of the invention

[0006] In order to solve the above technical problems, the present invention provides a propiconazole distillation method and device, which adopts a continuous production and purification process to avoid the static stage, thereby solving the problem of low production efficiency; by setting multiple distillation steps, the organic solvent and the product are recovered separately, thereby solving the problem of mixed distillation affecting the product concentration; by circulating distillation, the problem of product loss caused by incomplete distillation is avoided. It is specifically achieved by the following technical solutions:

[0007] The present invention discloses a propiconazole distillation device, comprising a mixing tank, the mixing tank is used to prepare a raw material mixed liquid, the outlet of the mixing tank is connected to the inlet of a filter tank through a pipeline, a filter layer is installed in the filter tank, and the outlet of the filter tank is connected to a separation mechanism through a pipeline installed with a first pipeline pump;

[0008] The separation mechanism includes a separation cylinder and ultrasonic vibration rods. A plurality of ultrasonic vibration rods are installed in the separation cylinder. The ultrasonic vibration rods can quickly separate the organic phase and the inorganic phase in the mixed liquid. The organic phase is transported to the first distillation mechanism through a pipeline, and the inorganic phase is transported to the mixing tank.

[0009] The first distillation mechanism includes a heat dissipation pipe, which is used to heat the mixed liquid. The heat dissipation pipe is arranged inside the distillation chamber. A feed pipe is installed at the bottom of the distillation chamber, and an exhaust pipe is installed at the top of the distillation chamber. The exhaust pipe is connected to the inlet of the cooling tower through a pipeline installed with an airflow meter.

[0010] The top of the side of the distillation chamber is connected to the inlet of the electric three-way valve, the first outlet of the electric three-way valve is connected to the inlet of the second distillation mechanism, and the second outlet of the electric three-way valve is connected to the feed pipe.

[0011] The second distillation mechanism has the same structure as the first distillation mechanism. The gas collected by the second distillation mechanism is transported to the second cooling tower, and the remaining liquid of the second distillation mechanism is transported to the mixing tank.

[0012] The first pipeline pump, the separation mechanism, the first distillation mechanism, and the second distillation mechanism are respectively connected to the controller signal.

[0013] Preferably, the first distillation mechanism further comprises a circulation cylinder, in which a first partition is installed, and the first partition seals and separates the circulation cylinder into two chambers, and the two chambers are respectively fixedly connected to two ends of the heat dissipation pipe.

[0014] The structure consisting of the distillation chamber, the feed pipe, the exhaust pipe, the airflow meter and the electric three-way valve is arranged in multiple groups along the length direction of the heat dissipation pipe, and a second partition is sealed between adjacent distillation chambers.

[0015] The second outlet of the electric three-way valve is fixedly connected to the next group of feed pipes through a circulation pipe, and the second outlet of the last group of electric three-way valves is fixedly connected to the inlet of the second pipeline pump through a pipeline equipped with a one-way valve, and the outlet of the second pipeline pump is fixedly connected to the first group of feed pipes.

[0016] The first outlet of each group of the electric three-way valves is communicated with the inlet of the second distillation mechanism through a pipeline.

[0017] The second pipeline pump and each group of the air flow meter and the electric three-way valve are respectively connected to the controller signal.

[0018] Preferably, the separation mechanism further comprises a pipeline port, the outlet of the filter tank is fixedly connected to the pipeline port via a pipeline equipped with the first pipeline pump, the pipeline port is fixedly connected to an annular pipe, and the annular pipe is fixedly connected to the separation cylinder via a plurality of diversion pipes.

[0019] An upper cylinder is installed on the top of the separation cylinder, a liquid level sensor is installed on the top of the upper cylinder, and the side of the upper cylinder is fixedly connected to the first liquid outlet pipe, and the first liquid outlet pipe is fixedly connected to the inlet of the second pipeline pump through a pipeline.

[0020] A lower cylinder is installed at the bottom of the separation cylinder, a second liquid outlet pipe is installed at the bottom of the lower cylinder, and the second liquid outlet pipe is connected with the mixing tank through a pipeline.

[0021] Preferably, the upper end surface of the lower cylinder is higher than the lower end surface of the separation cylinder and lower than the upper end surface of the ultrasonic vibration rod, and the ultrasonic vibration rod is located in the annular gap formed by the lower cylinder and the separation cylinder.

[0022] Preferably, the annular tube is an annular structure, and the annular tube is coaxially arranged with the separation cylinder.

[0023] Preferably, the pipeline opening is arranged tangentially to the annular tube.

[0024] Preferably, the cross-sectional area of ​​the diverter pipe gradually increases from the end connected to the annular pipe to the end connected to the separation cylinder.

[0025] Preferably, the heat dissipation pipe is a U-shaped pipe.

[0026] The present invention provides a propiconazole distillation method, which specifically comprises the following steps:

[0027] S1. Put the crude propiconazole and the organic solvent into a mixing tank and mix them evenly until the crude propiconazole is basically dissolved, then add clean water to wash and stir evenly to obtain a mixed solution.

[0028] S2. The mixed solution is transported to a filter tank for preliminary filtration to remove undissolved impurities.

[0029] S3, conveying the filtered mixed liquid to a separation mechanism to separate the organic phase and the inorganic phase, conveying the organic phase to a first distillation mechanism to distill the organic solvent, and conveying the inorganic phase to a mixing tank.

[0030] S4, the organic solvent obtained by distillation in step S3 is condensed through a first cooling tower and then transported to a mixing tank, and the remaining organic phase is transported to a second distillation mechanism for propiconazole distillation.

[0031] S5. The propiconazole obtained by distillation in step S4 is condensed and recovered through a second cooling tower to obtain a propiconazole distillation product, and the remaining organic phase is transported to a mixing tank.

[0032] After adopting the above technical solution, the beneficial effects of the present invention are:

[0033] 1. The ultrasonic vibrating rod in the separation mechanism can realize the rapid separation of the mixed organic phase and inorganic phase, avoiding the static step in the traditional process, greatly saving production time and improving production efficiency;

[0034] 2. Through stage distillation, the amount of gas evaporated by the detector at each stage of distillation is monitored to realize the degree of distillation, avoiding the problem of insufficient distillation or excessive distillation;

[0035] 3. By adjusting and controlling the amount of propiconazole distilled, the remaining amount of propiconazole in the organic phase can be accurately controlled to avoid product loss and excessive distillation affecting product purity;

[0036] 4. Through the recycling and distillation of the remaining inorganic phase, the effective ingredients in the product can be fully recovered, and the recycling of the inorganic phase and solvent effectively reduces the production cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0038] Figure 1 It is a structural schematic diagram of a propiconazole distillation device;

[0039] Figure 2 is a schematic structural diagram of a first distillation mechanism;

[0040] Figure 3 It is a structural schematic diagram of the separation mechanism;

[0041] Figure 4 for Figure 3 Stereoscopic image of

[0042] Figure 5 for Figure 3 Front cross-sectional view of .

[0043] Description of reference numerals:

[0044] 101-mixing tank, 102-filtering tank, 103-filtering layer, 104-first pipeline pump, 105-cooling tower;

[0045] 200-separation mechanism, 201-pipe opening, 202-annular pipe, 203-diverter pipe, 204-separation cylinder, 205-ultrasonic vibration rod, 206-upper cylinder, 207-liquid level sensor, 208-first liquid outlet pipe, 209-lower cylinder, 210-second liquid outlet pipe;

[0046] 300-first distillation mechanism, 301-circulation cylinder, 302-first baffle, 303-heat dissipation pipe, 304-distillation chamber, 305-second baffle, 306-feed pipe, 307-exhaust pipe, 308-air flow meter, 309-electric three-way valve, 310-check valve, 311-circulation pipe, 312-second pipeline pump;

[0047] 400 - second distillation mechanism, 500 - controller. DETAILED DESCRIPTION

[0048] The features and exemplary embodiments of various aspects of the present invention will be described in detail below. In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are only configured to explain the present invention and are not configured to limit the present invention. For those skilled in the art, the present invention can be implemented without the need for some of these specific details. The following description of the embodiments is only to provide a better understanding of the present invention by illustrating examples of the present invention.

[0049] The directional words appearing in the following description are all directions shown in the figures, and do not limit the specific structure of the present invention. In the description of the present invention, it should also be noted that, unless otherwise clearly specified and limited, the terms "installation" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected or indirectly connected. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to the specific circumstances.

[0050] The embodiment of the present invention provides a propiconazole distillation method and device, see Figures 1 to 5 The propiconazole distillation device includes a mixing tank 101, in which a stirrer is arranged for fully mixing the crude propiconazole, the organic solvent and water. The mixed liquid is transported to the bottom of the filter tank 102 through an outlet installed on the mixing tank 101. A filter layer 103 is fixedly installed in the middle of the filter tank 102 to separate the filter tank 102 into two independent areas, and is used to complete the filtration of the mixed liquid. The filtered mixed liquid is pumped to the separation mechanism 200 through a first pipeline pump 104.

[0051] The separation mechanism 200 includes a separation cylinder 204 and an ultrasonic vibration rod 205. The mixed liquid after the above filtration can be arranged in the separation cylinder 204. A plurality of ultrasonic vibration rods 205 are evenly installed along the circumference of the separation cylinder 204. The ultrasonic vibration rods 205 can promote the rapid separation of the organic phase and the inorganic phase in the mixed liquid. The separated organic phase passes through the first distillation mechanism 300 and the second distillation mechanism 400 in turn, and the inorganic phase is transported to the mixing tank 101 for recycling.

[0052] The first distillation mechanism 300 and the second distillation mechanism 400 have the same structure and are respectively used to complete the distillation of the organic solvent and propiconazole. The first distillation mechanism 300 includes a heat pipe 303, a distillation chamber 304, a feed pipe 306, an exhaust pipe 307, an airflow meter 308, and an electric three-way valve 309. The heat pipe 303 is provided with circulating hot steam for completing the heating of the mixed liquid. The heat pipe 303 is arranged inside the distillation chamber 304. The mixed liquid is placed in the distillation chamber 304. The feed pipe 306 is fixedly installed at the bottom of the distillation chamber 304, and the exhaust pipe 307 is fixedly installed at the top of the distillation chamber 304. The exhaust pipe 307 is fixedly connected to the air inlet of the cooling tower 105 through a pipeline equipped with the airflow meter 308, and the airflow meter 308 can detect the air flow rate.

[0053] The top of the side of the distillation chamber 304 is fixedly connected and communicated with the inlet of the electric three-way valve 309 , the first outlet of the electric three-way valve 309 is connected and communicated with the inlet of the second distillation mechanism 400 , and the second outlet of the electric three-way valve 309 is connected and communicated with the feed pipe 306 .

[0054] The first pipeline pump 104 , the separation mechanism 200 , the first distillation mechanism 300 , and the second distillation mechanism 400 are respectively connected to the controller 500 by signals.

[0055] Among them, the gases evaporated by the first distillation mechanism 300 and the second distillation mechanism 400 are cooled respectively through different cooling towers 105. The gas evaporated by the first distillation mechanism 300 is an organic solvent, which is condensed by the cooling tower 105 and then circulated to the mixing tank 101 for reuse. The gas evaporated by the second distillation mechanism 400 is propiconazole, which is condensed by the cooling tower 105 and then recovered as the final product.

[0056] Among them, after the mixed liquid passes through the separation mechanism 200 to separate the organic phase and the inorganic phase, the inorganic phase is directly transported to the mixing tank 101 for recycling, and the organic phase is first transported to the distillation chamber 304 through the feed pipe 306 to complete distillation. The gas after distillation is transported to the cooling tower 105 through the exhaust pipe 307 and the airflow meter 308 to complete condensation, and is recirculated to the mixing tank 101 as an organic solvent for reuse.

[0057] The heat dissipation tube 303 is a U-shaped tube, and a plurality of heat dissipation tubes 303 are evenly arranged and used together to complete the heating in the distillation chamber 304 .

[0058] The electric three-way valve 309 can only achieve communication between the inlet and one of the outlets, that is, when one of the outlets is opened, the other outlet is automatically closed.

[0059] When the air flow value detected by the airflow meter 308 is greater than the first preset value, the electric three-way valve 309 opens the second outlet; when the air flow value detected by the airflow meter 308 is less than or equal to the first preset value, the electric three-way valve 309 opens the first outlet.

[0060] The airflow meter 308 and the electric three-way valve 309 are respectively connected to the controller 500 by signals. The airflow meter 308 transmits the measurement data to the controller 500 , and the controller 500 adjusts the opening and closing of the electric three-way valve 309 according to the measurement data of the airflow meter 308 .

[0061] Among them, the purpose of fixing and connecting the top of the side of the distillation chamber 304 with the inlet of the electric three-way valve 309 is to transport the organic phase separated from the separation mechanism 200 to the distillation chamber 304, and after being heated by the heat pipe 303, since the organic phase in the distillation chamber 304 is circulating, there is a difference in the liquid flow temperature. At this time, the organic phase with a higher temperature is easier to float to the top of the distillation chamber 304 due to its lower density, and first completes the distillation and circulates to the next distillation chamber 304. The organic phase with a lower temperature is located below the distillation chamber 304 due to its higher density. After being heated, it gradually heats up, completes evaporation in this process and gradually flows to the top of the distillation chamber 304. Therefore, the above structure ensures that the concentration gradient of the solvent changes with the depth in the distillation chamber 304, which is conducive to the orderly distillation of the solvent.

[0062] In the above embodiment of the present invention, the crude propiconazole, organic solvent and water are first mixed in the mixing tank 101. After being fully mixed, the mixed liquid is transported to the filtering tank for preliminary filtration, and the filtered mixed liquid is transported to the separation mechanism 200.

[0063] Then, the organic phase and the inorganic phase of the mixed liquid are quickly separated in the separation mechanism 200, the inorganic phase is transported to the mixing tank 101 for recycling, and the organic phase is transported to the first distillation mechanism 300 to complete the distillation of the organic solvent. The organic solvent gas obtained by distillation is condensed through the cooling tower 105 and then transported to the mixing tank 101 for recycling.

[0064] During the distillation process, the flow rate of the distillation gas is measured by the airflow meter 308, and the degree of distillation completion is estimated by the flow value. When the airflow value detected by the airflow meter 308 is greater than the first preset value, it means that the distillation has not been completed. At this time, the electric three-way valve 309 opens the second outlet, and the undistilled organic phase is circulated and distilled in the distillation chamber 304 until the airflow value detected by the airflow meter 308 is less than or equal to the first preset value, indicating that the organic solvent in the organic phase is basically distilled. At this time, the electric three-way valve 309 opens the first outlet, and the organic phase in the distillation chamber 304 is transported to the second distillation mechanism 400 to complete the distillation of propiconazole.

[0065] The gas distilled by the second distillation mechanism 400 is condensed to obtain a propiconazole product. After the distillation of the second distillation mechanism 400 is completed, there is still some propiconazole residue in the remaining organic phase. Therefore, the remaining organic phase is transported to the mixing tank 101 for recycling to avoid the loss of the propiconazole component.

[0066] As another embodiment of the present invention, see Figure 2 On the basis of the above embodiment, the first distillation mechanism 300 also includes a circulation cylinder 301, a first partition 302, a second partition 305, a one-way valve 310, a circulation pipe 311, and a second pipeline pump 312. The two ends of the heat dissipation pipe 303 are respectively fixedly connected and communicated with the circulation cylinder 301. A horizontally arranged first partition 302 is fixedly installed in the circulation cylinder 301. The first partition 302 divides the circulation cylinder 301 into two independent chambers, one of which is fixedly connected to the first ends of a plurality of heat dissipation pipes 303, and the other is fixedly connected to the second ends of a plurality of heat dissipation pipes 303. Hot steam enters the heat dissipation pipe 303 through the first chamber, and is discharged to the outside through the second chamber after heat dissipation.

[0067] Several distillation chambers 304 are installed in sequence along the length direction of the heat dissipation pipe 303, and two adjacent distillation chambers 304 are sealed and separated by a second partition plate 305. Each distillation chamber 304 is connected in series through a circulation pipe 311, that is, the second outlet of the electric three-way valve 309 installed on the first group of distillation chambers 304 is fixedly connected and communicated with the feed pipe 306 installed on the second group of distillation chambers 304 through the circulation pipe 311, and the second outlet of the electric three-way valve 309 installed on the second group of distillation chambers 304 is fixedly connected and communicated with the feed pipe 306 installed on the third group of distillation chambers 304 through the circulation pipe 311. By analogy, the second outlet of the electric three-way valve 309 installed on the last group of distillation chambers 304 is fixedly connected and communicated with the inlet of the second pipeline pump 312 through a pipeline equipped with a one-way valve 310, the outlet of the second pipeline pump 312 is fixedly connected and communicated with the feed pipe 306 installed on the first group of distillation chambers 304, and the second pipeline pump 312 is signal-connected to the controller 500.

[0068] Among them, the structure composed of the distillation chamber 304, the feed pipe 306, the exhaust pipe 307, the airflow meter 308, and the electric three-way valve 309 is preferably 4 groups, and the airflow meter 308 and the electric three-way valve 309 in each group are respectively connected to the controller 500 signal.

[0069] Wherein, each circulation pipe 311 can be installed with a circulation pump to speed up the transmission of the organic phase between each distillation chamber 304 .

[0070] On the basis of the above-mentioned embodiments, this embodiment adds several groups of distillation chambers 304 so that the evaporant content in the organic phase in each distillation chamber 304 is different, thereby controlling the concentration of the evaporant in the organic phase more accurately.

[0071] First, the organic phase separated by the separation mechanism 200 is transported to the first group of distillation chambers 304 through the second pipeline pump 312 to complete distillation, and is measured by the first group of airflow meters 308 to determine whether the organic phase after the first distillation needs to be distilled for a second time. If so, the controller 500 controls the second outlet of the first group of electric three-way valves 309 to open, and transports the organic phase to the second group of distillation chambers 304 through the circulation pipe 311 to complete the second distillation. If not, the controller 500 controls the first outlet of the first group of electric three-way valves 309 to open, and transports the organic phase to the second distillation mechanism 400 to continue the distillation of propiconazole.

[0072] In order to fully utilize the multiple groups of distillation chambers 304 and more accurately control the concentration of evaporants in the organic phase, the controller 500 appropriately adjusts the pumping speed of the second pipeline pump 312 (i.e., by adjusting the flow rate of the organic phase entering the distillation chamber 304) so ​​that the gas flow value detected by the last group of gas flow meters 308 is less than or equal to the first preset value. Specifically, when the gas flow value detected by the third group of gas flow meters 308 is less than or equal to the first preset value, the fourth group of distillation chambers 304 does not participate in distillation, and the controller 500 controls the second pipeline pump 312 to pump the gas flow. 2 The pumping flow rate is increased so that the gas flow value detected by the third group of gas flow meters 308 is greater than the first preset value, and the fourth group of distillation chambers 304 begin to participate in distillation; when the gas flow value detected by the fourth group of gas flow meters 308 is greater than the first preset value, the organic phase needs to be re-distilled multiple times through the one-way valve 310 and the second pipeline pump 312, thereby reducing the distillation efficiency. Therefore, the controller 500 controls the second pipeline pump 312 to reduce the pumping flow rate so that the gas flow value detected by the fourth group of gas flow meters 308 is less than or equal to the first preset value.

[0073] In summary, by controlling the second pipeline pump 312 through the controller 500 to adjust the pumping flow, when the gas flow value detected by the third group of airflow meters 308 is greater than the first preset value and the gas flow value detected by the fourth group is less than or equal to the first preset value, each group of distillation chambers 304 is fully utilized, thereby achieving precise control of the components in the organic phase; in addition, unnecessary cyclic distillation processes are avoided, the efficiency of distillation is improved, and excessive distillation of the product to produce by-products is avoided, affecting product quality.

[0074] For further explanation of the present invention, see Figures 3 to 5 The separation mechanism 200 also includes a pipeline port 201, an annular pipe 202, a shunt pipe 203, an upper cylinder 206, a liquid level sensor 207, a first liquid outlet pipe 208, a lower cylinder 209, and a second liquid outlet pipe 210. The outlet of the filter tank 102 is fixedly connected and communicated with the first end of the pipeline port 201 through a pipeline installed with the first pipeline pump 104. The second end of the pipeline port 201 is fixedly connected and communicated with the outer side surface of the annular pipe 202. The inner side surface of the annular pipe 202 is evenly fixed along the circumferential direction and is communicated with the first ends of several shunt pipes 203. The second ends of several shunt pipes 203 are respectively fixedly connected and communicated with the outer side surface of the separation cylinder 204.

[0075] An upper cylinder 206 is coaxially fixed to the top of the separation cylinder 204, and a liquid level sensor 207 is fixedly installed on the top of the upper cylinder 206. The liquid level sensor 207 is used to detect the liquid level in the upper cylinder 206. The side of the upper cylinder 206 is fixedly connected and communicated with the first liquid outlet pipe 208, and the first liquid outlet pipe 208 is fixedly connected and communicated with the inlet of the second pipeline pump 312 through a pipeline.

[0076] The bottom of the separation cylinder 204 is coaxially fixed with the lower cylinder 209 , and the bottom of the lower cylinder 209 is fixedly connected and communicated with the second liquid outlet pipe 210 , and the second liquid outlet pipe 210 is communicated with the mixing tank 101 through a pipeline.

[0077] Among them, the annular tube 202 is an annular structure, the pipe port 201 is set tangent to the annular tube 202, and the cross-sectional area of ​​the diverter pipe 203 gradually increases from one end connected to the annular tube 202 to the end connected to the separation cylinder 204. The purpose of the above design is that when the mixed liquid enters the separation cylinder 204 through the pipe port 201, the annular tube 202, and the diverter pipe 203, its flow rate gradually slows down, which is conducive to phase separation after entering the separation cylinder 204.

[0078] Among them, the upper end surface of the lower cylinder 209 is higher than the lower end surface of the separation cylinder 204 and lower than the upper end surface of the ultrasonic vibration rod 205. The ultrasonic vibration rod 205 is located in the annular gap formed by the lower cylinder 209 and the separation cylinder 204. The purpose of this structure is to ensure that the mixed liquid transported into the separation cylinder 204 through the diversion pipe 203 has sufficient contact time with the ultrasonic vibration rod 205, thereby effectively realizing the separation of the organic phase and the inorganic phase.

[0079] In the above process, the working principle of the alternating positive and negative pressure cycles during the transmission of ultrasound is utilized; in the positive phase, the medium is squeezed to increase the original density of the medium, and in the negative phase, the medium molecules are sparse and discrete, and the medium density is reduced.

[0080] This periodic change causes strong vibration and cavitation effect inside the liquid, that is, a large number of tiny bubbles are generated and explode and split with the ultrasonic vibration. This extreme physical condition helps to destroy the interfacial balance between the organic phase and the inorganic phase, so that tiny gaps are generated between the two phases that were originally closely connected, making them easier to separate; the tiny bubbles exploded and split by the cavitation effect are affected by buoyancy, and adhere to the suspended particles of the organic phase during the rising process, further promoting the separation of the two phases; in addition, the strong vibration inside the liquid causes part of the energy generated to be converted into heat energy, resulting in local temperature rise inside the liquid, which helps to reduce the viscosity between the two phases and makes it easier to separate the two phases; the two phases that are easier to separate promote the convergence of the same phases and form stratification under the action of gravity.

[0081] This process avoids the static step in the traditional process and can quickly extract the organic phase from the mixed liquid, thus realizing the continuous and automated production of propiconazole, thereby greatly improving work efficiency.

[0082] The controller 500 controls the start and stop of the first pipeline pump 104 and the pumping speed of the first pipeline pump 104, thereby controlling the liquid level in the upper cylinder 206 to avoid incomplete separation of the organic phase and the inorganic phase due to too fast or too slow flow rate.

[0083] As a further explanation of the present invention, the present invention completes the distillation of propiconazole through the above-mentioned device, and the specific method steps are:

[0084] S1, put the crude propiconazole and the organic solvent into a mixing tank 101 and mix them evenly until the crude propiconazole is substantially completely dissolved, then add clean water for washing and stir evenly to obtain a mixed solution;

[0085] S2, transporting the mixed solution to the filter tank 102 to complete preliminary filtration, filtering and removing the impurities that cannot be dissolved;

[0086] S3, conveying the filtered mixed liquid to the separation mechanism 200 to separate the organic phase and the inorganic phase, conveying the upper organic phase to the first distillation mechanism 300 to distill the organic solvent, and conveying the lower inorganic phase to the mixing tank 101 for recycling;

[0087] S4, the organic solvent obtained by distillation in step S3 is condensed by the cooling tower 105 and then transported to the mixing tank 101 for recycling, and the remaining organic phase is transported to the second distillation mechanism 400 for propiconazole distillation;

[0088] S5. The propiconazole obtained by distillation in step S4 is condensed and recovered as a high-purity product through a cooling tower 105, and the remaining organic phase of the distillation is transported to the mixing tank 101 for recycling.

[0089] According to the embodiments of the present invention as described above, these embodiments do not describe all the details in detail, nor do they limit the invention to specific embodiments. Obviously, many modifications and changes can be made based on the above description. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can make good use of the present invention and the modified use based on the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A propiconazole distillation device, comprising a mixing tank (101), characterized in that: The mixing tank (101) is used to prepare a raw material mixed liquid, the outlet of the mixing tank (101) is connected to the inlet of the filtering tank (102) through a pipeline, a filter layer (103) is installed in the filtering tank (102), and the outlet of the filtering tank (102) is connected to the separation mechanism (200) through a pipeline installed with a first pipeline pump (104); The separation mechanism (200) comprises a separation cylinder (204) and ultrasonic vibration rods (205), wherein a plurality of ultrasonic vibration rods (205) are installed in the separation cylinder (204), and the ultrasonic vibration rods (205) are capable of quickly separating an organic phase and an inorganic phase in a mixed liquid, wherein the organic phase is transported to a first distillation mechanism (300) through a pipeline, and the inorganic phase is transported to the mixing tank (101); The first distillation mechanism (300) comprises a heat dissipation pipe (303), the heat dissipation pipe (303) is used to heat the mixed liquid, the heat dissipation pipe (303) is arranged inside the distillation chamber (304), a feed pipe (306) is installed at the bottom of the distillation chamber (304), an exhaust pipe (307) is installed at the top of the distillation chamber (304), and the exhaust pipe (307) is connected to the inlet of the cooling tower (105) through a pipeline installed with an airflow meter (308); The top of the side of the distillation chamber (304) is connected to the inlet of the electric three-way valve (309), the first outlet of the electric three-way valve (309) is connected to the inlet of the second distillation mechanism (400), and the second outlet of the electric three-way valve (309) is connected to the feed pipe (306); The second distillation mechanism (400) has the same structure as the first distillation mechanism (300), the gas collected by the second distillation mechanism (400) is transported to the second cooling tower (105), and the remaining liquid of the second distillation mechanism (400) is transported to the mixing tank (101); The first pipeline pump (104), the separation mechanism (200), the first distillation mechanism (300), and the second distillation mechanism (400) are respectively connected to the controller (500) via signals; The first distillation mechanism (300) further comprises a circulation cylinder (301), wherein a first partition (302) is installed in the circulation cylinder (301), and the first partition (302) seals and separates the circulation cylinder (301) into two chambers, wherein the two chambers are respectively fixedly connected to two ends of the heat dissipation pipe (303); The structure consisting of the distillation chamber (304), the feed pipe (306), the exhaust pipe (307), the airflow meter (308), and the electric three-way valve (309) is arranged in multiple groups along the length direction of the heat dissipation pipe (303), and a second partition plate (305) is sealed between adjacent distillation chambers (304); The second outlet of the electric three-way valve (309) is fixedly connected to the next group of feed pipes (306) through a circulation pipe (311), and the second outlet of the last group of electric three-way valves (309) is fixedly connected to the inlet of a second pipeline pump (312) through a pipeline equipped with a one-way valve (310), and the outlet of the second pipeline pump (312) is fixedly connected to the first group of feed pipes (306); The first outlet of each group of the electric three-way valves (309) is connected to the inlet of the second distillation mechanism (400) through a pipeline; The second pipeline pump (312) and each group of the airflow meter (308) and the electric three-way valve (309) are respectively connected to the controller (500) via signals.

2. The propiconazole distillation device according to claim 1, characterized in that: The separation mechanism (200) further comprises a pipeline port (201), the outlet of the filter tank (102) being fixedly connected to the pipeline port (201) via a pipeline equipped with the first pipeline pump (104), the pipeline port (201) being fixedly connected to an annular pipe (202), and the annular pipe (202) being fixedly connected to the separation cylinder (204) via a plurality of diverter pipes (203); An upper cylinder (206) is installed on the top of the separation cylinder (204), a liquid level sensor (207) is installed on the top of the upper cylinder (206), a side surface of the upper cylinder (206) is fixedly connected to a first liquid outlet pipe (208), and the first liquid outlet pipe (208) is fixedly connected to an inlet of a second pipeline pump (312) through a pipeline; A lower cylinder (209) is installed at the bottom of the separation cylinder (204), and a second liquid outlet pipe (210) is installed at the bottom of the lower cylinder (209). The second liquid outlet pipe (210) is connected to the mixing tank (101) through a pipeline.

3. The propiconazole distillation device according to claim 2, characterized in that: The upper end surface of the lower cylinder (209) is higher than the lower end surface of the separation cylinder (204) and lower than the upper end surface of the ultrasonic vibration rod (205); the ultrasonic vibration rod (205) is located in an annular gap formed by the lower cylinder (209) and the separation cylinder (204).

4. The propiconazole distillation device according to claim 2, characterized in that: The annular tube (202) is an annular structure, and the annular tube (202) and the separation cylinder (204) are coaxially arranged.

5. The propiconazole distillation device according to claim 2, characterized in that: The pipeline opening (201) is arranged tangentially to the annular tube (202).

6. The propiconazole distillation device according to claim 2, characterized in that: The cross-sectional area of ​​the flow dividing pipe (203) gradually increases from the end connected to the annular pipe (202) to the end connected to the separation cylinder (204).

7. The propiconazole distillation device according to claim 1, characterized in that: The heat dissipation pipe (303) is a U-shaped pipe.

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