Desolventizing device for pyraclostrobin production

Abstract

The utility model relates to the technical field of pesticide production, in particular to a desolventizing device for pyraclostrobin production, which comprises a heating component, a circulating spraying component and a condensation recovery component. Under the action of the circulating pump of the circulating spraying assembly, a synthetic product at the bottom in the desolventizing tower is led out and enters the spraying piece through the circulating pipeline to be sprayed downwards, the sprayed liquid is dispersed into small liquid drops, the contact area with the outside is increased, a small amount of ethanol in the liquid is promoted to be removed, and the desolventizing effect is improved. Meanwhile, the liquid drops sprayed downwards pass through a heating environment formed by the spiral coil pipe and are heated again, so that the ethanol is easier to escape, and the desolventizing effect of the ethanol is improved. According to the condensation recovery assembly, condensed ethanol can be divided into two paths, one path returns to the desolventizing tower for desolventizing treatment when the purity of the ethanol is unqualified, and the other path enters the ethanol recovery tank for recovery when the purity of the ethanol is qualified, so that the purity of the recovered ethanol is improved.

Description

Technical Field

[0001] This utility model relates to the field of pesticide production technology, specifically to a desolvation device for the production of pyraclostrobin. Background Technology

[0002] Pyraclostrobin is a broad-spectrum, highly effective methoxyacrylate fungicide, mainly used to control various fungal diseases on crops.

[0003] CN202310648956.1 discloses a process for synthesizing pyraclostrobin technical grade, which includes the following steps: Step 1: Reacting ATBT with chloroacetic anhydride to obtain CTBT; Step 2: Reacting AMP under alkaline conditions to obtain MPTBT; Step 3: Reacting MPTBT with chloroformate under alkaline conditions to obtain MPCPTBT; Step 4: Reacting MPCPTBT with sodium hydroxide in ethanol to obtain pyraclostrobin. The synthesis process of this invention features mild reaction conditions, short reaction time, high yield, and good environmental friendliness, significantly improving the synthesis efficiency of pyraclostrobin, reducing costs, and minimizing environmental pollution. The patent specifies that the amount of ethanol used in step 4 is 9-11 times the total amount of reactants. It is evident that ethanol is used in large quantities as a solvent in the actual production of pyraclostrobin. To facilitate subsequent purification, solvent removal from the synthesized product is necessary to reduce or remove the high solvent content. Current technology typically removes ethanol from the product in a solvent removal tower. The principle is based on the different boiling points of different substances; since ethanol has a lower boiling point, the ethanol is evaporated and recovered by controlling the heating temperature. However, this method has the following technical drawbacks:

[0004] (1) Because an excessive amount of ethanol was used in the synthesis of pyraclostrobin, the ethanol content in the product was relatively high. After being mixed with other products, it was not easy to separate and remove the ethanol under heating conditions, which increased the desolvation time.

[0005] (2) In the desolventizing process of the desolventizing tower, in the initial stage or when the process control is unstable, the light ethanol component at the top of the desolventizing tower will carry some impurities, which will affect the purity of the ethanol after condensation and recovery. Utility Model Content

[0006] To address the technical problem of difficult ethanol separation and the easy inclusion of impurities affecting purity during solvent extraction, this invention provides a solvent extraction device for pyraclostrobin production, which can effectively separate and remove ethanol with a high content in the synthetic product, improve the solvent extraction effect, and at the same time help improve the purity of the recovered ethanol.

[0007] This utility model provides a solvent removal device for the production of pyraclostrobin, including a solvent removal tower, a feed inlet connected to a feed pipe at the side of the solvent removal tower, a light phase component outlet at the top of the solvent removal tower, and a heavy phase component outlet at the bottom of the solvent removal tower, and further comprising:

[0008] The heating assembly includes a reboiler, the input of which is connected to the bottom of the desolventizing tower via a first pipeline, and the output of which is connected to the side of the desolventizing tower via a second pipeline.

[0009] The circulating spray assembly includes a spray element and a circulating pipeline. The spray element is located inside the descaling tower and fixed to the inner wall of the descaling tower. One end of the circulating pipeline is connected to the lower part of the descaling tower, and the other end is connected to the spray element. A circulating pump is installed on the circulating pipeline. A spiral coil is installed directly below the spray element. One end of the spiral coil is connected to a steam supply device through a steam input pipeline, and the other end of the spiral coil is connected to a steam recovery device through a steam output pipeline.

[0010] The condensation recovery assembly includes a condenser and an ethanol recovery tank. The heat medium input end of the condenser is connected to the light phase component outlet at the top of the desolvation tower via a third pipeline. The heat medium output end of the condenser is connected to a fifth pipeline via a fourth pipeline. One end of the fifth pipeline is connected to a circulation pipeline, and the other end of the fifth pipeline is connected to the feed inlet of the ethanol recovery tank.

[0011] Furthermore, the spraying component includes a spray housing with a spray cavity, and the lower end face of the spray housing is provided with a plurality of evenly distributed spray holes. The spray cavity is connected to the circulation pipeline. Its function is to allow the synthesis product transported from the circulation pipeline to be passed into the spray cavity and sprayed downward from the spray holes, thereby forming a uniform spraying effect.

[0012] Furthermore, the heavy phase component outlet at the bottom of the desolventizing tower is connected to a discharge pipe, which is equipped with a first valve to discharge the synthesis product after ethanol separation for further separation and purification.

[0013] Furthermore, a second valve is installed on the circulation pipeline.

[0014] Furthermore, the fourth pipeline is equipped with a water pump, a third valve, and a sampling port. The water pump provides power for the condensed ethanol, and the sampling port allows operators to take samples from the pipeline at any time for testing and processing to determine whether the purity of the recovered ethanol is up to standard.

[0015] Furthermore, a fourth valve and a fifth valve are installed on the fifth pipeline, with the fourth valve and the fifth valve located on both sides of the fourth pipeline, respectively.

[0016] The beneficial effects of this utility model are as follows:

[0017] (1) Under the action of the circulating pump, the synthesis product at the bottom of the desolventizing tower is drawn out through the circulating pipeline and sprayed downwards into the spraying part. After spraying, the liquid is dispersed into small droplets, which increases the contact area with the outside world and promotes the removal of a small amount of ethanol in the liquid. At the same time, the droplets sprayed downwards are heated again through the heating environment formed by the spiral coil, making it easier for ethanol to escape and improving the desolventizing effect of ethanol.

[0018] (2) This utility model can divide the condensed ethanol into two paths. One path is returned to the desolventizing tower for desolventizing when the ethanol purity is not up to standard, and the other path is entered into the ethanol recovery tank for recovery when the ethanol purity is up to standard, thereby improving the purity of the recovered ethanol. Attached Figure Description

[0019] To more clearly illustrate the technical solution of this utility model, the drawings used in the description will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of the present utility model.

[0021] Figure 2 This is a schematic diagram of the spray component structure according to a specific embodiment of this utility model.

[0022] In the diagram, 1-reboiler, 2-first pipeline, 3-second pipeline, 4-feed pipe, 5-steam input pipeline, 6-steam output pipeline, 7-spray component, 71-spray shell, 72-spray cavity, 73-spray hole, 8-desolventizing tower, 9-third pipeline, 10-spiral coil, 11-second valve, 12-circulation pump, 13-first valve, 14-discharge pipe, 15-circulation pipeline, 16-fifth pipeline, 17-fourth valve, 18-sampling port, 19-condenser, 20-water pump, 21-fourth pipeline, 22-fifth valve, 23-third valve, 24-ethanol recovery tank. Detailed Implementation

[0023] To make the objectives, features, and advantages of this utility model more apparent and understandable, the technical solutions of this utility model will be clearly and completely described below with reference to the accompanying drawings of the specific embodiments. Obviously, the embodiments described below are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this patent, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this patent.

[0024] Example 1

[0025] Combination Figure 1 This utility model provides a solvent removal device for the production of pyraclostrobin, including a solvent removal tower 8, a feed inlet connected to a feed pipe 4 at the side of the solvent removal tower 8, a light phase component outlet at the top of the solvent removal tower 8, a heavy phase component outlet at the bottom of the solvent removal tower 8, a discharge pipe 14 connected to the heavy phase component outlet, and a first valve 13 on the discharge pipe 14. The device also includes:

[0026] The heating assembly includes a reboiler 1, the input end of which is connected to the bottom of the desolventizing tower 8 via a first pipeline 2, and the output end of which is connected to the side of the desolventizing tower 8 via a second pipeline 3. The heating assembly is used to heat the synthesis product at the bottom of the desolventizing tower 8.

[0027] The circulating spray assembly includes a spray element 7 and a circulating pipeline 15. The spray element 7 is located inside the descaling tower 8 and fixed to the inner wall of the descaling tower 8. Figure 2 The spraying component 7 includes a spraying shell 71 with a spraying cavity 72. The lower end face of the spraying shell 71 is provided with a plurality of evenly distributed spraying holes 73. The spraying cavity 72 is connected to one end of the circulation pipeline 15, and the other end of the circulation pipeline 15 is connected to the lower part of the desolvation tower 8. The circulation pipeline 15 is provided with a circulation pump 12 and a second valve 11. A spiral coil 10 is provided directly below the spraying component 7. One end of the spiral coil 10 is connected to a steam supply device through a steam input pipeline 5, and the other end of the spiral coil 10 is connected to a steam recovery device through a steam output pipeline 6.

[0028] The condensation recovery assembly includes a condenser 19 and an ethanol recovery tank 24. The heat medium input end of the condenser 19 is connected to the light phase component outlet at the top of the desolvation tower 8 via a third pipeline 9. The heat medium output end of the condenser 19 is connected to a fifth pipeline 16 via a fourth pipeline 21. The fourth pipeline 21 is equipped with a water pump 20, a third valve 23, and a sampling port 18. One end of the fifth pipeline 16 is connected to a circulation pipeline 15, and the other end of the fifth pipeline 16 is connected to the inlet of the ethanol recovery tank 24. The fifth pipeline 16 is equipped with a fourth valve 17 and a fifth valve 22, which are located on both sides of the fourth pipeline 21.

[0029] The workflow of this utility model is as follows:

[0030] After synthesis, the mixed liquid containing pyraclostrobin is fed into the desolventizing tower 8 through the feed pipe 4. The reboiler 1 is started to circulate and heat the mixed liquid until it reaches the boiling point of ethanol, 80~85℃. Some ethanol begins to escape from the light component outlet at the top of the tower and enters the condenser 19 for condensation. At this initial stage, the ethanol contains more impurities. The fifth valve 22 is closed, and the fourth valve 17 and the third valve 23 are opened. The unqualified ethanol is returned to the tower for desolventizing treatment. The condensed ethanol is sampled through the sampling port 18. When the purity is qualified, the fourth valve 17 is closed and the fifth valve 22 is opened to recover the ethanol into the ethanol recovery tank 24.

[0031] In the later stage of solvent removal, the second valve 11 is opened and the circulation pump 12 is started. The mixed liquid in the tower is drawn out through the circulation pipeline 15 and sprayed downwards into the spray unit 7. After being sprayed, the liquid is dispersed into small droplets, increasing the contact area with the outside world and promoting the removal of a small amount of ethanol in the liquid. At this time, steam is introduced into the spiral coil 10. The downward sprayed droplets are heated again through the heating environment formed by the spiral coil 10, making it easier for ethanol to escape and improving the solvent removal effect of ethanol.

[0032] The above description of the disclosed embodiments enables those skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A pyraclostrobin production desolventizing device, comprising a desolventizing tower, a feed pipe connected to a side feed inlet of the desolventizing tower, a light phase component outlet provided at a top of the desolventizing tower, and a heavy phase component outlet provided at a bottom of the desolventizing tower, characterized in that, Also comprising: a heating assembly, including a reboiler, an input end of the reboiler being connected to a bottom part of the desolventizing tower through a first pipeline, and an output end of the reboiler being connected to a side part of the desolventizing tower through a second pipeline; a circulating spraying assembly, including a spraying member and a circulating pipeline, the spraying member being located inside the desolventizing tower and fixed to an inner wall of the desolventizing tower, one end of the circulating pipeline being connected to a lower part of the desolventizing tower, and the other end of the circulating pipeline being connected to the spraying member, a circulating pump being arranged on the circulating pipeline, a spiral coil being arranged right below the spraying member, one end of the spiral coil being connected to a steam supply device through a steam input pipeline, and the other end of the spiral coil being connected to a steam recovery device through a steam output pipeline; a condensing and recovering assembly, including a condenser and an ethanol recovery tank, a hot medium input end of the condenser being connected to a light phase component outlet at a top part of the desolventizing tower through a third pipeline, a hot medium output end of the condenser being connected to a fourth pipeline through a fifth pipeline, one end of the fifth pipeline being connected to the circulating pipeline, and the other end of the fifth pipeline being connected to a feed inlet of the ethanol recovery tank.

2. The pyraclostrobin production desolventizing device according to claim 1, wherein The spraying member includes a spraying shell with a spraying cavity, a lower end surface of the spraying shell being provided with a plurality of spraying holes which are uniformly distributed, and the spraying cavity being communicated with the circulating pipeline.

3. The pyraclostrobin production desolventizing device according to claim 1, wherein A heavy phase component outlet at the bottom part of the desolventizing tower is connected to a discharge pipe, and the discharge pipe is provided with a first valve.

4. The pyraclostrobin production desolventizing device according to claim 1, wherein The circulating pipeline is provided with a second valve.

5. The pyraclostrobin production desolventizing device according to claim 1, wherein The fourth pipeline is provided with a water pump, a third valve and a sampling port.

6. The pyraclostrobin production desolventizing device according to claim 1, wherein The fifth pipeline is provided with a fourth valve and a fifth valve, and the fourth valve and the fifth valve are respectively arranged on two sides of the fourth pipeline.

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