Pesticide fluorination reaction crystallization device

Abstract

The utility model discloses a pesticide fluorination reaction crystallization device which comprises a reaction kettle body, a shell is arranged on the outer wall of the reaction kettle body, an ultrasonic generator is installed on one side of the circumferential outer wall of the shell, transducers are arranged at the bottom of the reaction kettle body in an annular array mode, and the ultrasonic generator is installed on one side of the circumferential outer wall of the shell. The reaction kettle body is provided with a stirring assembly used for stirring materials in the reaction kettle body, a feeding assembly used for feeding seed crystals into the reaction kettle body, and a driving assembly used for driving the stirring assembly and the feeding assembly. According to the reaction kettle, fine crystal nucleuses can be broken, excessive crystal nucleuses in the reaction kettle body can be reduced, so that the crystals grow more uniformly, the mass transfer efficiency is enhanced, the cooling process is more uniform, the phenomenon of local supercooling and superheating is avoided, stable growth of the crystals is facilitated, and the crystals are promoted to grow to a larger particle size; and subsequent solid-liquid separation and screening are facilitated.

Description

Technical Field

[0001] This utility model relates to the technical field of pesticide fluorination reaction crystallization equipment, specifically a pesticide fluorination reaction crystallization device. Background Technology

[0002] In the field of pesticide synthesis, fluorination reaction is a key process for preparing fluorinated pesticides. The efficiency of the crystallization process and the quality of the crystals directly affect the purity of the product and the subsequent separation cost. Traditional crystallization processes usually use a single stirring or cooling method, which has problems such as uneven crystal particle size distribution, easy aggregation, and difficulty in accurately controlling the nucleation rate.

[0003] A search revealed that patent publication number CN210674295U discloses a reactor device for vacuum concentration and cooling crystallization, comprising a reactor body, an outer water bath jacket, an inner oil bath jacket, a variable frequency motor, an anchor-type stirring paddle, a vacuum system, and a circulating water bath. The reactor body has a feed inlet and a vacuum port at the top, and a discharge port at the bottom. The outer surface of the reactor body is sequentially wrapped with the inner oil bath jacket and the outer water bath jacket. The variable frequency motor is located above the reactor body, and the bottom of the variable frequency motor has a motor output shaft that extends into the interior of the reactor body, with an anchor-type stirring paddle installed at its lower end. The vacuum port is connected to the vacuum system via a conduit. The outer water bath jacket has a water inlet and a water outlet on both sides, which are connected to the circulating water bath via conduits. This invention enables continuous concentration and cooling crystallization operations within the same reactor.

[0004] In practical use, existing pesticide fluorination reaction crystallization devices typically require the crystallization process to go through stages such as nucleation, growth, and aging. During the low-temperature crystallization stage, the solution is highly supersaturated. If there is a lack of effective dispersion methods, it is easy to cause explosive nucleation, forming small crystals or agglomerates, which affects filtration efficiency and product purity. Therefore, a pesticide fluorination reaction crystallization device was designed. Utility Model Content

[0005] In view of the defects or deficiencies of the existing pesticide fluorination reaction crystallization device, the purpose of this utility model is to provide a pesticide fluorination reaction crystallization device that can break up small crystal nuclei, reduce the number of excessive crystal nuclei inside the reaction vessel, avoid local overcooling and overheating, promote stable crystal growth and promote crystal growth to a larger particle size, which facilitates subsequent solid-liquid separation and sieving.

[0006] To achieve the above-mentioned objectives, the present invention adopts the following technical solution:

[0007] This utility model provides a pesticide fluorination reaction crystallization device, including a reaction vessel body, an outer shell provided on the outer wall of the reaction vessel body, an ultrasonic generator installed on one side of the circumferential outer wall of the outer shell, transducers arranged in a ring array at the bottom of the reaction vessel body, a stirring assembly for stirring the material inside the reaction vessel body, a feeding assembly for feeding seed crystals into the reaction vessel body, and a driving assembly for driving the stirring assembly and the feeding assembly.

[0008] Preferably, a cooling medium flow cavity is provided between the inner wall of the outer shell and the outer wall of the reactor body. An outlet pipe is provided above one side of the outer circumferential wall of the outer shell, and an inlet pipe is provided below the other side of the outer circumferential wall of the outer shell. Both the outlet pipe and the inlet pipe are connected to the cooling medium flow cavity.

[0009] Preferably, the feeding assembly is provided with a shell, which is located on one side of the top of the reactor body, and the interior of the shell is connected to the interior of the reactor body. The interior of the shell is provided with a rotating shaft and a spiral blade, and the spiral blade is located below the outer wall of the rotating shaft.

[0010] Preferably, the other end of the rotating shaft passes through a sealed bearing at the center of the top of the housing and is connected to a single-groove pulley. A feeding pipe is provided above the outer wall of one side of the housing, and a valve body is provided on the feeding pipe.

[0011] Preferably, the stirring assembly is provided with a stirring paddle, which is located inside the reactor body. The stirring paddle is installed on the outer wall of the stirring shaft, and the top end of the stirring shaft passes through the sealed bearing at the center of the top end of the reactor body and extends to the outside to connect with the double groove pulley.

[0012] Preferably, the drive assembly is equipped with a geared motor, which is installed on the other side of the top of the reactor body. A single-groove pulley is installed on the output shaft of the geared motor. The single-groove pulley on the geared motor is connected to a double-groove pulley on the stirring shaft via a transmission belt. The double-groove pulley on the stirring shaft is connected to a single-groove pulley on the rotating shaft via a transmission belt.

[0013] Compared with existing technologies, one or more of the above technical solutions have the following beneficial effects:

[0014] In this invention, through a series of coordinated structural designs, when the equipment is undergoing cooling and crystallization, the operator adds a pesticide fluorination reaction solution to the inside of the reactor. In the initial stage of cooling and crystallization, the operator activates an ultrasonic generator to generate a large number of tiny cavitation bubbles in the solution using the cavitation effect. This breaks up the small crystal nuclei, preventing the crystals from becoming too small and hindering subsequent solid-liquid separation and sieving. This promotes more uniform crystal growth, enhances mass transfer efficiency in the solution, and makes the cooling process more uniform, avoiding local overcooling and overheating. This is beneficial for stable crystal growth and promotes crystal growth to a larger particle size, facilitating subsequent solid-liquid separation and sieving.

[0015] In this invention, through a series of coordinated structural arrangements, in the later stage of cooling and crystallization, the operator turns off the ultrasonic generator and starts the geared motor on the drive assembly. The drive assembly drives the stirring assembly to stir the solution inside the reactor at a low speed. The low-speed stirring of the solution inside the reactor by the stirring assembly helps to shape the growth direction and morphology of the crystals, making the crystals more regular. The low-speed rotation of the stirring assembly can also promote the diffusion of solutes in the solution, so that the solutes required for crystal growth can reach the crystal surface in a timely manner, thereby improving the crystallization efficiency.

[0016] In this invention, through a series of coordinated structural arrangements, when the stirring component rotates at low speed, it drives the rotating shaft on the feeding component to rotate. When the rotating shaft rotates, it drives the spiral blades to rotate. When the spiral blades rotate, seed crystals can be introduced into the reactor body. Introducing seed crystals into the reactor body can provide a ready-made surface for crystal growth, guide crystal growth, make crystal growth more orderly, and facilitate the formation of crystals with larger particle sizes, which further facilitates subsequent solid-liquid separation and sieving. Attached Figure Description

[0017] The accompanying drawings, which form part of this specification, are used to provide a further understanding of this utility model. The illustrative embodiments of this utility model and their descriptions are used to explain this utility model and do not constitute an improper limitation of this utility model.

[0018] Figure 1 This is a schematic diagram of the overall three-dimensional structure of this utility model. Figure 1 .

[0019] Figure 2 This is a schematic diagram of the overall three-dimensional structure of this utility model. Figure 2 .

[0020] Figure 3 This is a cross-sectional view of the entire utility model.

[0021] Figure 4 This is a schematic diagram of the feeding component of this utility model.

[0022] In the picture:

[0023] 100. Reactor body;

[0024] 200. Outer casing; 210. Inlet pipe; 220. Outlet pipe;

[0025] 300. Feeding assembly; 310. Housing; 320. Feeding pipe; 330. Rotating shaft; 340. Spiral blade;

[0026] 400. Stirring assembly;

[0027] 500. Driver components;

[0028] 600. Ultrasonic generator;

[0029] 700. Transducer. Detailed Implementation

[0030] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0031] It should be noted that the following detailed description is exemplary and intended to provide further explanation of the present invention. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0032] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of exemplary embodiments according to the invention. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0033] like Figure 1-4 As shown, a pesticide fluorination reaction crystallization apparatus includes a reaction vessel 100, an outer shell 200 on the outer wall of the reaction vessel 100, an ultrasonic generator 600 installed on one side of the circumferential outer wall of the outer shell 200, transducers 700 arranged in a ring array at the bottom of the reaction vessel 100, a stirring assembly 400 for stirring the materials inside the reaction vessel 100, a feeding assembly 300 for feeding seed crystals into the reaction vessel 100, and a driving assembly 500 for driving the stirring assembly 400 and the feeding assembly 300.

[0034] A cooling medium flow cavity is provided between the inner wall of the outer shell 200 and the outer wall of the reactor body 100. An outlet pipe 220 is provided above one side of the outer wall of the outer shell 200, and an inlet pipe 210 is provided below the other side of the outer wall of the outer shell 200. Both the outlet pipe 220 and the inlet pipe 210 are connected to the cooling medium flow cavity. An external cooling medium conveying device inputs the cooling medium from the inlet pipe 210 into the cooling medium flow cavity. The cooling medium in the cooling medium flow cavity is discharged from the outlet pipe 220. When the cooling medium flows in the cooling medium flow cavity, it can cool the solution inside the reactor body 100.

[0035] The feeding assembly 300 is provided with a housing 310, which is located on one side of the top of the reactor body 100. The interior of the housing 310 is connected to the interior of the reactor body 100. The interior of the housing 310 is provided with a rotating shaft 330 and a spiral blade 340, and the spiral blade 340 is located below the outer wall of the rotating shaft 330.

[0036] The other end of the rotating shaft 330 passes through the sealed bearing at the center of the top of the housing 310 and is connected to the single-groove pulley. A feeding pipe 320 is provided above the outer wall of one side of the housing 310, and a valve body is provided on the feeding pipe 320.

[0037] The stirring assembly 400 is equipped with a stirring paddle, which is located inside the reactor body 100. The stirring paddle is installed on the outer wall of the stirring shaft. The top end of the stirring shaft passes through the sealed bearing at the center of the top end of the reactor body 100 and extends to the outside to connect with the double groove pulley.

[0038] A geared motor is installed on the drive assembly 500, which is mounted on the other side of the top of the reactor body 100. A single-groove pulley is installed on the output shaft of the geared motor. The single-groove pulley on the geared motor is connected to a double-groove pulley on the stirring shaft via a transmission belt. The double-groove pulley on the stirring shaft is connected to a single-groove pulley on the rotating shaft 330 via a transmission belt. When the geared motor starts, it drives the single-groove pulley on its output shaft to rotate. When the single-groove pulley on the geared motor rotates, it drives the double-groove pulley on the stirring shaft to rotate via the transmission belt. When the double-groove pulley rotates, it drives the stirring shaft to rotate. When the stirring shaft rotates, it drives the stirring paddle to rotate. When the double-groove pulley rotates, it drives the single-groove pulley on the rotating shaft 330 to rotate via the transmission belt. When the single-groove pulley on the rotating shaft 330 rotates, it drives the rotating shaft 330 to rotate. When the rotating shaft 330 rotates, it causes the spiral blade 340 to rotate.

[0039] Working Principle: When in use, connect the external power supply. During the cooling and crystallization operation, the operator adds a pesticide fluorination reaction solution to the reactor body 100. In the initial stage of cooling and crystallization, the operator activates the ultrasonic generator 600. Utilizing the cavitation effect, a large number of tiny cavitation bubbles are generated in the solution, which can break up small crystal nuclei. This avoids the situation where too many small crystal nuclei result in small crystal particle sizes, which would hinder subsequent solid-liquid separation and sieving. It promotes more uniform crystal growth and enhances the mass transfer efficiency in the solution, making the cooling process more uniform and avoiding localized overcooling or overheating. This is beneficial for stable crystal growth and promotes crystal growth to a larger particle size, facilitating subsequent solid-liquid separation and sieving. In the later stage of cooling and crystallization, the operator turns off the ultrasonic generator 600 and starts the geared motor on the drive assembly 500. The drive assembly 500 will then drive the agitator. The stirring component 400 provides low-speed stirring of the solution inside the reactor body 100. This low-speed stirring helps to influence the growth direction and morphology of the crystals, resulting in more regular crystals. The low-speed rotation of the stirring component 400 also promotes the diffusion of solutes in the solution, ensuring that the solutes required for crystal growth can reach the crystal surface in a timely manner, thus improving crystallization efficiency. When the stirring component 400 rotates at low speed, it drives the rotating shaft 330 on the feeding component 300 to rotate. The rotation of the rotating shaft 330 drives the spiral blades 340 to rotate, which can introduce seed crystals into the reactor body 100. Introducing seed crystals into the reactor body 100 provides a ready-made surface for crystal growth, guiding crystal growth and making crystal growth more orderly. This is conducive to forming crystals with larger particle sizes, further facilitating subsequent solid-liquid separation and sieving.

[0040] The above description is merely a preferred embodiment of this utility model and is not intended to limit the invention. For those skilled in the art, various modifications and variations can be made to this invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this invention should be included within the protection scope of this invention.

Claims

1. A pesticide fluorination reaction crystallization apparatus, comprising a reaction vessel (100), characterized in that: An outer shell (200) is provided on the outer wall of the reactor body (100). An ultrasonic generator (600) is installed on one side of the circumferential outer wall of the outer shell (200). A transducer (700) is arranged in a ring array at the bottom of the reactor body (100). A stirring assembly (400) for stirring the material inside the reactor body (100) is provided on the reactor body (100). A feeding assembly (300) for feeding seed crystals into the reactor body (100) is provided on the reactor body (100). A driving assembly (500) for driving the stirring assembly (400) and the feeding assembly (300) is provided on the reactor body (100).

2. The pesticide fluorination reaction crystallization apparatus according to claim 1, characterized in that: A cooling medium flow cavity is provided between the inner wall of the outer shell (200) and the outer wall of the reactor body (100). A liquid outlet pipe (220) is provided above one side of the outer circumferential outer wall of the outer shell (200), and a liquid inlet pipe (210) is provided below the other side of the outer circumferential outer wall of the outer shell (200). Both the liquid outlet pipe (220) and the liquid inlet pipe (210) are connected to the cooling medium flow cavity.

3. The pesticide fluorination reaction crystallization apparatus according to claim 1, characterized in that: The feeding assembly (300) is provided with a housing (310), which is located on one side of the top of the reactor body (100), and the interior of the housing (310) is connected to the interior of the reactor body (100). The interior of the housing (310) is provided with a rotating shaft (330) and a spiral blade (340), and the spiral blade (340) is located below the outer wall of the rotating shaft (330).

4. The pesticide fluorination reaction crystallization apparatus according to claim 3, characterized in that: The other end of the rotating shaft (330) passes through the sealed bearing at the center of the top of the housing (310) and is connected to the single-groove pulley. A feeding pipe (320) is provided above the outer wall of one side of the housing (310), and a valve body is provided on the feeding pipe (320).

5. The pesticide fluorination reaction crystallization apparatus according to claim 1, characterized in that: The stirring assembly (400) is provided with a stirring paddle, which is located inside the reactor body (100). The stirring paddle is installed on the outer wall of the stirring shaft. The top end of the stirring shaft passes through the sealed bearing at the center of the top end of the reactor body (100) and extends to the outside to connect with the double groove pulley.

6. The pesticide fluorination reaction crystallization apparatus according to claim 1, characterized in that: The drive assembly (500) is equipped with a geared motor, which is installed on the other side of the top of the reactor body (100). A single-groove pulley is installed on the output shaft of the geared motor. The single-groove pulley on the geared motor is connected to a double-groove pulley on the stirring shaft via a transmission belt. The double-groove pulley on the stirring shaft is connected to a single-groove pulley on the rotating shaft (330) via a transmission belt.

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