Recovery device for butyl acetate in azoxystrobin production

Abstract

The utility model provides a device for recovering butyl acetate in azoxystrobin production. The device comprises a distillation kettle, a condenser, a low-boiling-point substance collecting tank, a butyl acetate collecting tank and a vacuum pump, a gas phase outlet in the top of the distillation kettle is communicated with a gas phase inlet of a condenser, a liquid phase outlet of the condenser is connected with a liquid outlet pipe, the outlet end of the liquid outlet pipe is respectively connected with a first liquid conveying pipe and a second liquid conveying pipe, the first liquid conveying pipe is communicated with a low-boiling-point substance collecting tank, and the second liquid conveying pipe is communicated with a butyl acetate collecting tank; the top of the butyl acetate collecting tank is connected with a vacuum pump; the first infusion tube is provided with a first valve, and the second infusion tube is provided with a second valve. The method provided by the utility model realizes efficient recovery of butyl acetate.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of distillation equipment, and particularly relates to a butyl acetate recovery device in azoxystrobin production. BACKGROUND

[0002] Azoxystrobin is a kind of methoxy acrylate fungicide. In the production process of azoxystrobin, butyl acetate is used as a crystallizing agent when azoxystrobin is crystallized, and butyl acetate solvent containing impurities is obtained after the crystallization is completed.

[0003] If the low-quality butyl acetate solvent is directly discharged, not only the butyl acetate resource will be wasted, but also the environmental protection will be burdened. If the low-quality butyl acetate solvent is reused, the azoxystrobin product yield will be low and the quality will be poor due to the high impurity content. CONTENT OF THE UTILITY MODEL

[0004] The present application provides a butyl acetate recovery device in azoxystrobin production to solve the above problems mentioned in the background.

[0005] The present application provides a butyl acetate recovery device in azoxystrobin production, which comprises a distillation kettle, a condenser, a low-boiling substance collecting tank, a butyl acetate collecting tank and a vacuum pump.

[0006] The gas phase outlet at the top of the distillation kettle is communicated with the gas phase inlet of the condenser, the liquid phase outlet of the condenser is connected with a liquid outlet pipe, the outlet end of the liquid outlet pipe is respectively connected with a first liquid inlet pipe and a second liquid inlet pipe, the first liquid inlet pipe is communicated with the low-boiling substance collecting tank, the second liquid inlet pipe is communicated with the butyl acetate collecting tank, and the top of the butyl acetate collecting tank is connected with the vacuum pump.

[0007] A first valve is arranged on the first liquid inlet pipe, and a second valve is arranged on the second liquid inlet pipe.

[0008] Optionally, a stirring unit is arranged in the distillation kettle, and the stirring unit comprises a motor, a connecting shaft and a stirring paddle.

[0009] The motor is arranged at the top of the distillation kettle, one end of the connecting shaft is connected with the output end of the motor, the other end of the connecting shaft vertically extends into the distillation kettle, the stirring paddle is arranged on the outer side of the connecting shaft and is symmetrically arranged about the center of the connecting shaft, a plurality of through holes are arranged in the lower part of the plate surface of the stirring paddle, and the sectional area of the through holes is 15-30% of the sectional area of the stirring paddle.

[0010] Optionally, the angle between the plate surface of the stirring paddle and the vertical direction is 10-25 degrees.

[0011] Optionally, a scraping plate is also vertically arranged in the distillation kettle, one side of the scraping plate in the vertical direction is connected with the end of the plurality of stirring paddles away from the connecting shaft, and the other side of the scraping plate in the vertical direction is in contact with the inner wall of the distillation kettle.

[0012] Optionally, a first installation groove is formed in the end of the stirring paddle away from the connecting shaft, a second installation groove is formed in the side of the scraping plate close to the stirring paddle, and the first installation groove and the second installation groove are fixedly connected with a spring.

[0013] Optionally, a temperature sensor is installed in the distillation kettle.

[0014] Optionally, a pressure sensor is installed in the distillation kettle.

[0015] The recovery device for butyl acetate in azoxystrobin production provided in the application realizes the recovery of butyl acetate, and has the following beneficial effects compared with the prior art:

[0016] (1) The low-boiling alcohol and water in the low-quality butyl acetate are first evaporated through normal pressure distillation to achieve the purpose of preliminary impurity removal, and then the butyl acetate solution is evaporated through the opening of the vacuum pump for decompression distillation of the distillation kettle to achieve the purpose of butyl acetate recovery, thereby avoiding the waste of butyl acetate resources. At the same time, after the low-quality butyl acetate is removed by the recovery device provided in the application, high-quality butyl acetate is obtained, which is helpful for the crystallization of azoxystrobin when it is used in azoxystrobin crystallization, thereby improving the quality of azoxystrobin. At the same time, the low-boiling substances are removed through normal pressure distillation, and then the butyl acetate is evaporated through decompression distillation. In the operation process, not only the energy consumption is saved and the recovery cost is reduced, but also the discharge of butyl acetate waste liquid is greatly reduced by recovering butyl acetate, which has good environmental benefits.

[0017] (2) A plurality of through holes are formed in the lower part of the stirring paddle surface. The plurality of through holes help a part of the material to collide with the stirring paddle and another part of the material to pass through the through holes during stirring, thereby improving the shearing efficiency of the stirring paddle on the material, making the stirring of the material more uniform, intensifying the turbulent flow of the material, and thereby facilitating the upward movement of the material vapor, thereby improving the distillation efficiency and the recovery efficiency and quality of butyl acetate. The cross-sectional area of the through hole is 15-30% of the stirring paddle. In this way, not only the distillation efficiency is improved, but also the stress area of the stirring paddle is ensured to avoid the reduction of the stirring intensity of the material caused by too many through holes.

[0018] (3) The material attached to the inner wall of the distillation kettle during the distillation process is scraped off in time by the scraping plate. The stirring paddle and the scraping plate are connected by the spring. The spring has elastic deformation. This setting transmits the pressure between the scraping plate and the inner wall of the distillation kettle to the spring during movement, so that the spring deforms elastically. Such elastic connection can avoid the wear of the scraping plate and the inner wall of the distillation kettle compared with the rigid connection between the stirring paddle and the scraping plate, and is conducive to the long-term stable operation of the device.

[0019] (4) The recovery device provided in the application has simple structure and convenient operation, and can be widely promoted in the industry. BRIEF DESCRIPTION OF DRAWINGS

[0020] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 A schematic diagram of the structure of a device for recovering butyl acetate in the production of azoxystrobin according to an embodiment of this application;

[0022] Figure 2 This is a schematic diagram of the structure of a stirring unit provided in one embodiment of this application;

[0023] Figure 3 This is a schematic diagram showing the connection between the scraper and the mixing blade according to an embodiment of this application;

[0024] Figure 4 A schematic diagram of a device for recovering butyl acetate in the production of azoxystrobin, provided in another embodiment of this application;

[0025] Explanation of reference numerals in the attached figures:

[0026] 1: Distillation vessel; 2: Condenser; 3: Low-boiling-point collection tank; 4: Butyl acetate collection tank; 5: Vacuum pump; 6: Spring; 7: Temperature sensor; 8: Pressure sensor; 110: Motor; 120: Connecting shaft; 130: Stirring paddle; 131: Through hole; 132: First mounting groove; 140: Scraper; 141: Second mounting groove; 210: Liquid outlet pipe; 220: First delivery pipe; 221: First valve; 230: Second delivery pipe; 231: Second valve. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application are described clearly and completely below. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort are also within the scope of protection of this application.

[0028] like Figure 1 As shown, this application provides a device for recovering butyl acetate in the production of azoxystrobin, comprising: a distillation kettle 1, a condenser 2, a low-boiling matter collection tank 3, a butyl acetate collection tank 4, and a vacuum pump 5.

[0029] The gas phase outlet at the top of the distillation kettle 1 is communicated with the gas phase inlet of the condenser 2, the liquid phase outlet of the condenser 2 is connected with a liquid outlet pipe 210, the outlet end of the liquid outlet pipe 210 is respectively connected with a first liquid inlet pipe 220 and a second liquid inlet pipe 230, the first liquid inlet pipe 220 is communicated with the low-boiling substance collecting tank 3, the second liquid inlet pipe 230 is communicated with the butyl acetate collecting tank 4, and the top of the butyl acetate collecting tank 4 is connected with a vacuum pump 5;

[0030] The first liquid inlet pipe 220 is provided with a first valve 221, and the second liquid inlet pipe 230 is provided with a second valve 231.

[0031] Specifically, low-quality butyl acetate is input into the distillation kettle 1, and the low-quality butyl acetate is heated (heated by a jacket, a heating coil or a heating pipe, which is not limited in the application), while the first valve 221 is opened, the second valve 231 and the vacuum pump 5 are closed, and the low-quality butyl acetate is subjected to normal pressure distillation, so that the alcohol and water with low boiling points in the low-quality butyl acetate are evaporated, the alcohol and water vapor enter the condenser 2 from the gas phase outlet at the top of the distillation kettle 1 for condensation, and the alcohol and water in liquid phase are obtained and output from the liquid outlet pipe 210 and input into the low-boiling substance collecting tank 3 through the first liquid inlet pipe 220, so as to remove the low-boiling substances in the low-quality butyl acetate. After the low-boiling substance is evaporated, the first valve 221 is closed, and the second valve 231 and the vacuum pump 5 are opened, so that the distillation kettle 1 is vacuumized by the vacuum pump 5, so that the distillation kettle 1 is in a negative pressure state, and the low-quality butyl acetate is subjected to reduced pressure distillation, so that butyl acetate is evaporated, and the reduced pressure distillation is beneficial to the vaporization of butyl acetate. The butyl acetate vapor enters the condenser 2 through the gas phase outlet at the top, is condensed to obtain liquid butyl acetate, is output from the liquid outlet pipe 210, and is collected into the butyl acetate collecting tank 4 through the second liquid inlet pipe 230, so as to achieve the purpose of purifying and recycling butyl acetate, and the recycled butyl acetate is used as a crystallizing agent in the azoxystrobin crystallization process. After the reduced pressure distillation is completed, the high-boiling substances remaining in the distillation kettle 1 are discharged from the kettle bottom discharge port as hazardous waste.

[0032] The application realizes the recycling of butyl acetate, the low-boiling alcohol and water in the low-quality butyl acetate are evaporated through normal pressure distillation, so as to achieve the purpose of preliminary impurity removal, then the distillation kettle is vacuumized by opening the vacuum pump, so that the butyl acetate solution is evaporated through reduced pressure distillation, so as to achieve the purpose of recycling butyl acetate, which avoids the waste of butyl acetate resources, and at the same time, after the low-quality butyl acetate is removed by the recycling device provided in the application, high-quality butyl acetate is obtained, which is helpful for the crystallization of azoxystrobin when it is used in the azoxystrobin crystallization, thereby improving the quality of azoxystrobin. At the same time, the low-boiling substances are removed through normal pressure distillation, and then the butyl acetate is evaporated through reduced pressure distillation, which not only saves energy consumption and reduces the recycling cost in the operation process, but also the device provided in the application has a simple structure and is easy to operate.

[0033] AsFigure 2 As shown in the figure, optionally, a stirring unit is arranged in the distillation kettle 1, and the stirring unit comprises a motor 110, a connecting shaft 120 and stirring paddles 130.

[0034] The motor 110 is arranged at the top of the distillation kettle 1, one end of the connecting shaft 120 is connected with the output end of the motor 110, the other end of the connecting shaft 120 vertically extends into the distillation kettle 1, and the stirring paddles 130 are arranged on the outer side of the connecting shaft 120 and are symmetrically arranged about the center of the connecting shaft 120. A plurality of through holes 131 are arranged on the lower part of the plate surface of the stirring paddles 130, and the cross-sectional area of the through holes 131 is 15-30% of the plate surface area of the stirring paddles 130.

[0035] Specifically, the stirring unit is used for stirring the material in the distillation kettle 1 during the distillation process, so as to improve the heating efficiency and uniformity of the low-quality butyl acetate, thereby helping the evaporation of the material. The motor 110 provides power to drive the connecting shaft 120 to rotate, and the stirring paddles 130 are arranged on the outer side of the connecting shaft 120. The connecting shaft 120 drives the stirring paddles 130 to rotate, and the stirring paddles 130 agitate the low-quality butyl acetate, which is conducive to the rapid heating and uniform heating of the low-quality butyl acetate, thereby improving the evaporation efficiency of the material. The stirring paddles 130 are symmetrically arranged about the center of the connecting shaft 120, which is conducive to uniform stress on each stirring paddle 130 and stable operation of the entire recovery device.

[0036] A plurality of through holes 131 are arranged on the lower part of the plate surface of the stirring paddles 130, which is conducive to the collision of a part of the material with the stirring paddles 130 and the passing of another part of the material through the through holes 131 during the stirring process. This improves the shearing efficiency of the stirring paddles on the material, makes the stirring of the material more uniform, and intensifies the turbulent flow of the material, thereby facilitating the upward movement of the material vapor, improving the distillation efficiency, and improving the recovery efficiency and quality of the butyl acetate. The sum of the cross-sectional areas of the plurality of through holes 131 is 15-30% of the plate surface area of the stirring paddles 130, which not only improves the distillation efficiency, but also ensures the stress area of the stirring paddles 130, avoiding excessive through holes 131 that reduce the stirring intensity of the material.

[0037] Optionally, the angle between the plate surface of the stirring paddles 130 and the vertical direction is 10-25°.

[0038] Specifically, this not only achieves the purpose of stirring the material, but also reduces the operating load of the motor 110.

[0039] As shown in the figure, Figure 2 Optionally, a scraper 140 is also vertically arranged in the distillation kettle 1, one side of the scraper 140 in the vertical direction is connected with one end of the plurality of stirring paddles 130 away from the connecting shaft 120, and the other side of the scraper 140 in the vertical direction is in contact with the inner wall of the distillation kettle 1.

[0040] Specifically, the scraper 140 is used to scrape off the material attached to the inner wall of the distillation kettle 1 in time during the distillation process. One side of the scraper 140 in the vertical direction is connected with the end of the plurality of stirring paddles 130 away from the connecting shaft 120, and the other side of the scraper 140 in the vertical direction is connected with the inner wall of the distillation kettle 1. In this way, when the stirring unit is running, the stirring paddles 130 can drive the scraper 140 to rotate at the same time, so as to scrape the inner wall of the distillation kettle 1, thereby avoiding the material from sticking to the wall.

[0041] As shown in Figure 2 and Figure 3 optionally, the end of the stirring paddle 130 away from the connecting shaft 120 is provided with a first mounting groove 132, and the side of the scraper 140 close to the stirring paddle 130 is provided with a second mounting groove 141 corresponding to the first mounting groove 132, and the first mounting groove 132 and the second mounting groove 141 are fixedly connected with the spring 6.

[0042] Specifically, the end of the stirring paddle 130 is provided with the first mounting groove 132, and the side of the scraper 140 close to the stirring paddle 130 is provided with the second mounting groove 141 at a horizontal position corresponding to the first mounting groove 132. One end of the spring 6 is fixedly connected with the first mounting groove 132, and the other end of the spring 6 is fixedly connected with the second mounting groove 141. The stirring paddle 130 and the scraper 140 are connected through the spring 6. The spring 6 has elastic deformation. In this way, the pressure between the scraper 140 and the inner wall of the distillation kettle 1 during movement is transmitted to the spring 6, so that the spring 6 is elastically deformed. Compared with the rigid connection between the stirring paddle 130 and the scraper 140, the elastic connection can avoid the abrasion between the scraper 140 and the inner wall of the distillation kettle 1, and is conducive to the long-term stable operation of the device.

[0043] As shown in Figure 4 optionally, the distillation kettle 1 is provided with the temperature sensor 7.

[0044] Specifically, the temperature sensor 7 is used to detect the temperature of the material in the distillation kettle 1 in real time, which helps the operator to observe whether the internal temperature reaches the design temperature in time and to adjust in time.

[0045] As shown in Figure 4 optionally, the distillation kettle 1 is provided with the pressure sensor 8.

[0046] Specifically, the pressure sensor 8 is used to detect the pressure of the material in the distillation kettle 1 in real time, and the frequency of the vacuum pump 5 is adjusted through the reading of the pressure sensor 8, so that the distillation kettle 1 maintains a set pressure value, which is conducive to the stable operation of the recovery device.

[0047] The technical scheme of the present application will be described in detail below with specific examples.

[0048] The recovery device for butyl acetate in the production of azoxystrobin in this embodiment has the following operation process during specific work:

[0049] The low-quality butyl acetate is input into the distillation kettle 1, and the low-quality butyl acetate is heated through the jacket, while the first valve 221 is opened, the second valve 231 and the vacuum pump 5 are closed, the motor 110 is opened, the connecting shaft 120 is driven to rotate, the stirring paddle 130 is driven to rotate by the connecting shaft 120, the low-quality butyl acetate is stirred by the stirring paddle 130, and the low-quality butyl acetate is subjected to atmospheric distillation, so that the alcohol and water with lower boiling points in the low-quality butyl acetate are evaporated, the alcohol and water vapor enter the condenser 2 through the top gas phase outlet of the distillation kettle 1, are condensed to obtain liquid alcohol and water, and are output through the liquid outlet pipe 210, input into the low-boiling substance collection tank 3 through the first liquid inlet pipe 220, and the purpose of removing the low-boiling substances in the low-quality butyl acetate is achieved.

[0050] After the temperature exceeds 100℃, the evaporation of the low-boiling substances is completed, the material in the distillation kettle 1 is cooled to 80℃, the first valve 221 is closed, and the second valve 231 and the vacuum pump 5 are opened, so that the distillation kettle 1 is vacuumized by the vacuum pump 5, and the distillation kettle 1 is in a negative pressure state (vacuum degree-80Kpa), the low-quality butyl acetate is subjected to reduced pressure distillation, and the butyl acetate is evaporated, which is conducive to the vaporization of the butyl acetate. The butyl acetate vapor enters the condenser 2 through the top gas phase outlet and is condensed to obtain liquid butyl acetate, which is output through the liquid outlet pipe 210 and input into the butyl acetate collection tank 4 through the second liquid inlet pipe 230, so that the purpose of purifying and recycling the butyl acetate is achieved, and the recycled butyl acetate is used as a crystallization agent in the azoxystrobin crystallization process. In the reduced pressure distillation process, the material in the distillation kettle 1 is continuously heated through the jacket, and when the temperature sensor 7 shows that the temperature is equal to 95℃, the reduced pressure distillation operation is stopped, and the remaining high-boiling substances in the distillation kettle 1 are discharged from the kettle bottom discharge port as hazardous waste.

[0051] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, and are not limited thereto; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that the technical solutions described in the foregoing embodiments can be modified, or some or all of the technical features can be replaced by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A device for recovering butyl acetate in azoxystrobin production, characterized by, The utility model relates to a butyl acetate production device, including: A distillation kettle (1), a condenser (2), a low boiling point substance collecting tank (3), a butyl acetate collecting tank (4) and a vacuum pump (5); The gas phase outlet of the top of the distillation kettle (1) is communicated with the gas phase inlet of the condenser (2), the liquid phase outlet of the condenser (2) is connected with a liquid outlet pipe (210), the outlet end of the liquid outlet pipe (210) is connected with a first liquid conveying pipe (220) and a second liquid conveying pipe (230) respectively, the first liquid conveying pipe (220) is communicated with the low boiling point substance collecting tank (3), the second liquid conveying pipe (230) is communicated with the butyl acetate collecting tank (4), and the top of the butyl acetate collecting tank (4) is connected with the vacuum pump (5); A first valve (221) is arranged on the first liquid conveying pipe (220), and a second valve (231) is arranged on the second liquid conveying pipe (230).

2. The device for recovering butyl acetate in production of azoxystrobin according to claim 1, characterized by, A stirring unit is arranged in the distillation kettle (1), and the stirring unit comprises a motor (110), a connecting shaft (120) and stirring paddles (130); The motor (110) is arranged at the top of the distillation kettle (1), one end of the connecting shaft (120) is connected with the output end of the motor (110), the other end of the connecting shaft (120) vertically extends into the distillation kettle (1), the stirring paddles (130) are arranged on the outer side of the connecting shaft (120) and are symmetrically arranged about the center of the connecting shaft (120), a plurality of through holes (131) are formed in the lower part of the plate surface of the stirring paddles (130), and the cross-sectional area of the plurality of through holes (131) is 15-30% of the stirring paddles (130).

3. The device for recovering butyl acetate in production of azoxystrobin according to claim 2, characterized by, The angle between the plate surface of the stirring paddles (130) and the vertical direction is 10-25 degrees.

4. The device for recovering butyl acetate in production of azoxystrobin according to claim 3, characterized by, A scraper (140) is also vertically arranged in the distillation kettle (1), one side of the scraper (140) in the vertical direction is connected with one end of the plurality of stirring paddles (130) away from the connecting shaft (120), and the other side of the scraper (140) in the vertical direction is in contact connection with the inner wall of the distillation kettle (1).

5. The device for recovering butyl acetate in production of azoxystrobin according to claim 4, characterized by, A first mounting groove (132) is formed in the end of the stirring paddles (130) away from the connecting shaft (120), a second mounting groove (141) is formed in the side of the scraper (140) close to the stirring paddles (130), and a spring (6) is fixedly connected between the first mounting groove (132) and the second mounting groove (141).

6. The device for recovering butyl acetate in production of azoxystrobin according to claim 1, characterized by, A temperature sensor (7) is installed in the distillation kettle (1).

7. The device for recovering butyl acetate in production of azoxystrobin according to any one of claims 1 to 6, characterized in that, A pressure sensor (8) is installed in the distillation kettle (1).

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