A device for efficiently removing dimethyl sulfide from an intermediate of tebuconazole epoxy
By using a thin-film evaporator for continuous distillation, the problem of low efficiency in traditional batch distillation is solved, achieving efficient separation of dimethyl sulfide, protecting heat-sensitive materials, and improving the purity and yield of tebuconazole intermediate epoxide.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- LIAONING ZHONGHUI BIOTECHNOLOGY CO LTD
- Filing Date
- 2025-08-11
- Publication Date
- 2026-07-21
AI Technical Summary
Traditional batch distillation in the process of removing dimethyl sulfide from tebuconazole intermediate epoxide is inefficient, has a long cycle, is prone to decomposition of heat-sensitive materials, and results in poor product purity.
The effects or results that can be achieved by using a thin-film evaporator for continuous distillation, combined with precise control of a pneumatic regulating valve and a temperature sensor, are as described above.
It improves distillation efficiency, shortens material residence time, reduces the risk of decomposition of heat-sensitive materials, and improves product purity and yield.
Smart Images
Figure CN224523974U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of chemical production equipment technology, and in particular to a device for the efficient removal of dimethyl sulfide from tebuconazole intermediate epoxy. Background Technology
[0002] 2-[2-(4-chlorophenyl)ethyl]-2-(1,1-dimethylethyl)ethylene oxide (hereinafter referred to as epoxy) is produced by reacting the intermediate 2-[2-(4-chlorophenyl)ethyl]-2-(1,1-dimethylethyl)-4-methyl-2-pentanone (hereinafter referred to as pentanone) with dimethyl sulfate using dimethyl sulfide as a solvent. After the reaction, a large amount of dimethyl sulfide remains in the system, requiring dedimethyl sulfide removal treatment. The traditional removal method involves stirring and heating in an enamel-lined reactor, followed by intermittent operation through steps such as feeding, heating for solvent removal, and discharging. The problem with this method is low operating efficiency, which severely restricts the output of epoxy. This paper presents a highly efficient dimethyl sulfide removal device for epoxy.
[0003] Thin-film evaporators are a new type of high-efficiency, energy-saving falling-film evaporator. They have superior performance characteristics such as high heat transfer coefficient (high evaporation intensity), short material residence time, wide applicable viscosity range, and high operational flexibility. The main principle is that after the material enters the evaporator, it is forced to form a film by the agitation of the hanging plates on the rotor. The heat source exchanges heat with the liquid through the cylinder wall, the liquid film boils, and the secondary steam is vaporized and discharged after the entrained droplets are removed by the film trap. The concentrated liquid is released from the bottom outlet.
[0004] To address the low efficiency of dimethyl sulfide removal from epoxy resins caused by traditional batch distillation, a high-efficiency dimethyl sulfide removal device for epoxy resins is proposed. This device employs a thin-film evaporator for continuous distillation, which significantly improves distillation efficiency, increases processing capacity, and accelerates dimethyl sulfide removal compared to traditional batch distillation. It effectively evaporates and separates low-boiling-point dimethyl sulfides from epoxy intermediates, thereby improving product purity and protecting heat-sensitive materials. The short residence time of materials within the thin-film evaporator, coupled with precise temperature control, reduces the risk of prolonged thermal decomposition, polymerization, or deterioration of the tebuconazole intermediate epoxy resin at high temperatures, thus improving the yield and quality of the target product. Utility Model Content
[0005] This invention provides a highly efficient device for removing dimethyl sulfide from tebuconazole intermediates, which solves the problems of low efficiency, long cycle, easy decomposition of heat-sensitive materials, low separation efficiency and poor product purity caused by traditional batch distillation.
[0006] The present invention provides the following solution to the above-mentioned technical problems: A high-efficiency device for removing dimethyl sulfide from tebuconazole intermediate epoxy, comprising a transfer tank, a transfer pump, a thin-film evaporator, a first receiving tank, a condenser, a second receiving tank, a feed pipe, a first discharge pipe, and a second discharge pipe. The transfer tank, the transfer pump, the feed pipe, and the thin-film evaporator are connected in sequence. The lower end of the thin-film evaporator is connected to the first receiving tank through the first discharge pipe, and the upper end of the thin-film evaporator is connected to the second receiving tank through the second discharge pipe. A condenser is installed on the second discharge pipe.
[0007] Based on the above technical solution, the present invention can be further improved as follows.
[0008] Furthermore, the transfer tank is equipped with a float level gauge, the transfer tank is loaded with epoxy containing dimethyl sulfide, and the thin-film evaporator continuously distills the epoxy containing dimethyl sulfide.
[0009] Furthermore, the float level gauge detects the liquid level in the transfer tank and shuts off the transfer pump when the liquid level is low to prevent the transfer pump from running dry and being damaged. This avoids the risk of dry burning, coking, or equipment damage caused by interruption of the feed to the thin film evaporator, and ensures the safe and stable operation of the system.
[0010] Furthermore, the thin-film evaporator is equipped with a pneumatic regulating valve, a temperature sensor, and a pressure sensor.
[0011] Furthermore, when the pressure sensor detects that the pressure in the thin-film evaporator is greater than 0.1M, the pneumatic regulating valve and the transfer pump are shut off to prevent the thin-film evaporator from overpressure due to blockage, poor condensation, or excessive steam, thus avoiding serious safety accidents such as equipment explosion and material leakage, and protecting the safety of personnel and equipment.
[0012] Furthermore, the pneumatic regulating valve is connected to the steam supply pipeline. The pneumatic regulating valve regulates the steam input flow of the thin film evaporator to achieve precise control of the heating power of the thin film evaporator. Combined with the temperature sensor, it ensures the temperature stability of the distillation process. This is crucial for the efficient and stable removal of dimethyl sulfide and the prevention of thermal decomposition of epoxy intermediates, thereby improving product quality and yield.
[0013] Furthermore, the condenser condenses the dimethyl sulfide distilled and vaporized by the thin-film evaporator, and the feed pipe is equipped with a feed flow meter to ensure that the dimethyl sulfide is fully condensed into liquid, which is convenient for collection and recovery in the No. 2 receiving tank. This prevents the dimethyl sulfide vapor from entering the environment and causing pollution and safety risks. Dimethyl sulfide is flammable and has a foul odor, which improves the purity of the epoxy after the target product is de-dimethyl sulfide removed.
[0014] Furthermore, the thin-film evaporator, receiving tank No. 1, condenser, and receiving tank No. 2 can be set up in two sets. The feed pipe is equipped with a three-way valve that connects to the two sets of evaporation components respectively. The device can be configured with two independent evaporation-condensation-receiving units. By operating in parallel, the overall production capacity of the device can be significantly improved. While one system is running, the other can be cleaned, maintained, or kept on standby, achieving near-continuous production or meeting different production needs. If one system fails, the other can continue to operate, reducing the risk of production interruption.
[0015] This invention provides a highly efficient device for removing dimethyl sulfide from tebuconazole intermediate epoxy, which has the following advantages:
[0016] 1. It can achieve efficient and continuous removal by using a thin-film evaporator for continuous distillation. The thin-film evaporator has the characteristics of high heat transfer efficiency, short material heating time, high evaporation intensity, and can handle high viscosity materials. This is significantly more efficient than the traditional batch distillation, with a large processing capacity (3000L / H) and faster removal of dimethyl sulfide.
[0017] 2. It can effectively improve separation efficiency and product purity. The special structure and efficient heat transfer of the thin film evaporator, combined with optimized temperature control (by regulating steam through a pneumatic regulating valve), can effectively evaporate and separate low-boiling-point dimethyl sulfide from the epoxy intermediate. The dimethyl sulfide vapor at the top is fully condensed and recovered by a special condenser, ensuring that the residual amount of dimethyl sulfide in the epoxy intermediate collected at the bottom (No. 1 receiving tank) is extremely low, thereby improving product purity.
[0018] 3. It can protect heat-sensitive materials. The material residence time in the thin film evaporator is short, and through precise temperature control (pneumatic regulating valve and temperature sensor), the risk of tebuconazole intermediate (epoxy) being decomposed, polymerized or deteriorated by prolonged heating at high temperature is greatly reduced, thereby improving the yield and quality of the target product.
[0019] The above description is merely an overview of the technical solution of this utility model. In order to better understand the technical means of this utility model and to implement it according to the contents of the specification, the preferred embodiments of this utility model are described in detail below with reference to the accompanying drawings. The specific implementation methods of this utility model are given in detail in the following embodiments and their accompanying drawings. Attached Figure Description
[0020] The accompanying drawings, which are included to provide a further understanding of the present invention and form part of this application, illustrate exemplary embodiments of the present invention and, together with the description thereof, serve to explain the present invention and do not constitute an undue limitation thereof. In the drawings:
[0021] Figure 1 A schematic diagram of a high-efficiency dimethyl sulfide removal device for tebuconazole intermediate epoxy is provided in one embodiment of this utility model;
[0022] Figure 2 This is a schematic diagram of a high-efficiency dedimethyl sulfide removal device for tebuconazole intermediate epoxy provided in one embodiment of the present invention, which is configured with two independent evaporation-condensation-receiving units.
[0023] The attached diagram lists the components represented by each number as follows:
[0024] 1. Transfer tank; 2. Transfer pump; 3. Thin-film evaporator; 4. No. 1 receiving tank; 5. Condenser; 6. No. 2 receiving tank; 7. Feed pipe; 8. Pneumatic regulating valve; 9. Feed flow meter; 10. No. 1 discharge pipeline; 11. No. 2 discharge pipeline; 12. Temperature sensor; 13. Pressure sensor; 14. Float level gauge. Detailed Implementation
[0025] The principles and features of this utility model are described below with reference to the accompanying drawings. The examples given are for illustrative purposes only and are not intended to limit the scope of this utility model. The utility model is described more specifically in the following paragraphs by way of example with reference to the accompanying drawings. The advantages and features of this utility model will become clearer from the following description and claims. It should be noted that the drawings are all in a very simplified form and use non-precise proportions, and are only used to facilitate and clarify the illustration of the embodiments of this utility model.
[0026] Unless otherwise defined, 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. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.
[0027] As shown in the figure, a high-efficiency epoxy dedimethyl sulfide removal device for tebuconazole intermediates includes a transfer tank 1, a transfer pump 2, a thin-film evaporator 3, a first receiving tank 4, a condenser 5, a second receiving tank 6, a feed pipe 7, a first discharge pipe 10, and a second discharge pipe 11. The transfer tank 1, the transfer pump 2, the feed pipe 7, and the thin-film evaporator 3 are connected in sequence. The lower end of the thin-film evaporator 3 is connected to the first receiving tank 4 through the first discharge pipe 10, and the upper end of the thin-film evaporator 3 is connected to the second receiving tank 6 through the second discharge pipe 11. The second discharge pipe 11 is equipped with a condenser 5.
[0028] Preferably, the transfer tank 1 is equipped with a float level gauge 14, the transfer tank 1 is loaded with epoxy containing dimethyl sulfide, and the thin film evaporator 3 continuously distills the epoxy containing dimethyl sulfide.
[0029] Preferably, the float level gauge 14 detects the liquid level of the transfer tank 1 and shuts off the transfer pump 2 when the liquid level is low to prevent the transfer pump 2 from running dry and being damaged, avoid the risk of dry burning, coking or equipment damage caused by interruption of feeding to the thin film evaporator 3, and ensure the safe and stable operation of the system.
[0030] Preferably, the thin-film evaporator 3 is equipped with a pneumatic regulating valve 8, a temperature sensor 12, and a pressure sensor 13.
[0031] Preferably, when the pressure sensor 13 detects that the pressure of the thin film evaporator 3 is greater than 0.1M, the pneumatic regulating valve 8 and the transfer pump 2 are closed to prevent the thin film evaporator from overpressure due to blockage, poor condensation, excessive steam, etc., and to avoid serious safety accidents such as equipment explosion and material leakage, thus protecting the safety of personnel and equipment.
[0032] Preferably, the pneumatic regulating valve 8 is connected to the steam supply pipeline. The pneumatic regulating valve 8 regulates the steam input flow of the thin film evaporator 3 to achieve precise control of the heating power of the thin film evaporator. Combined with the temperature sensor, it ensures that the temperature of the distillation process is stable. This is crucial for the efficient and stable removal of dimethyl sulfide and the prevention of thermal decomposition of epoxy intermediates, thereby improving product quality and yield.
[0033] Preferably, the condenser 5 condenses the dimethyl sulfide vaporized by the thin-film evaporator 3, and the feed pipe 7 is equipped with a feed flow meter 9 to ensure that the dimethyl sulfide is fully condensed into liquid, which is convenient for collection and recovery in the No. 2 receiving tank. This prevents the dimethyl sulfide vapor from entering the environment and causing pollution and safety risks. Dimethyl sulfide is flammable and has a foul odor, so this method improves the purity of the epoxy after the target product is de-dimethyl sulfide removed.
[0034] Preferably, the thin-film evaporator 3, the first receiving tank 4, the condenser 5, and the second receiving tank 6 can be set in two sets. The feed pipe 7 is equipped with a three-way valve that is connected to the two sets of evaporation components respectively. The device can be configured with two independent evaporation-condensation-receiving units. By operating in parallel, the overall capacity of the device can be significantly improved. One system is running while the other can be cleaned, maintained, or kept on standby, achieving near-continuous production or meeting different production needs. If one system fails, the other can continue to operate, reducing the risk of production interruption.
[0035] The specific working principle and usage method of this utility model are as follows:
[0036] During normal thin-film distillation, condenser 5 and pneumatic regulating valve 8 are turned on. After the thin-film evaporator 3 is preheated, transfer pump 2 and feed pipe 7 are turned on. Epoxy containing dimethyl sulfide in transfer tank 1 is pumped into thin-film evaporator 3 through feed flow meter 9, which controls the feed flow rate at 3000 L / H. Epoxy enters receiving tank 4 from the bottom of thin-film evaporator 3 through discharge line 10. The vaporized dimethyl sulfide is condensed by condenser 5 from the top and enters receiving tank 6 through discharge line 11.
[0037] The above description is merely a preferred embodiment of this utility model and is not intended to limit the utility model in any way. Those skilled in the art can readily implement this utility model based on the accompanying drawings and the above description. However, any modifications, alterations, or variations made by those skilled in the art without departing from the scope of the utility model's technical solution, utilizing the disclosed technical content, are equivalent embodiments of this utility model. Furthermore, any equivalent changes, alterations, or variations made to the above embodiments based on the essential technology of this utility model are still within the protection scope of this utility model's technical solution.
Claims
1. A high-efficiency device for removing dimethyl sulfide from tebuconazole intermediate epoxy, comprising a transfer tank (1), a transfer pump (2), a thin-film evaporator (3), a first receiving tank (4), a condenser (5), a second receiving tank (6), a feed pipe (7), a first discharge line (10), and a second discharge line (11), characterized in that: The transfer tank (1), transfer pump (2), feed pipe (7), and thin film evaporator (3) are connected in sequence. The lower end of the thin film evaporator (3) is connected to the first receiving tank (4) through the first discharge pipeline (10), and the upper end of the thin film evaporator (3) is connected to the second receiving tank (6) through the second discharge pipeline (11). The second discharge pipeline (11) is equipped with a condenser (5).
2. The device for efficient removal of dimethyl sulfide from tebuconazole intermediate epoxy according to claim 1, characterized in that, The transfer tank (1) is equipped with a float level gauge (14), the transfer tank (1) is loaded with epoxy containing dimethyl sulfide, and the thin film evaporator (3) continuously distills the epoxy containing dimethyl sulfide.
3. The device for efficient removal of dimethyl sulfide from tebuconazole intermediate epoxy according to claim 2, characterized in that, The float level gauge (14) detects the liquid level of the transfer tank (1) and shuts off the transfer pump (2) when the liquid level is low.
4. The high-efficiency dimethyl sulfide removal device for tebuconazole intermediate epoxy according to claim 1, characterized in that, The thin-film evaporator (3) is equipped with a pneumatic regulating valve (8), a temperature sensor (12), and a pressure sensor (13).
5. The device for efficient removal of dimethyl sulfide from tebuconazole intermediate epoxy according to claim 4, characterized in that, The pressure sensor (13) detects that the pneumatic regulating valve (8) and the transfer pump (2) are closed when the pressure of the thin film evaporator (3) is greater than 0.1M.
6. The device for efficient removal of dimethyl sulfide from tebuconazole intermediate epoxy according to claim 5, characterized in that, The pneumatic regulating valve (8) is connected to the steam supply pipeline and regulates the steam input flow of the thin film evaporator (3).
7. The device for efficient removal of dimethyl sulfide from tebuconazole intermediate epoxy according to claim 1, characterized in that, The condenser (5) condenses the thin film evaporator (3) and distills and vaporizes the dimethyl sulfide. The feed pipe (7) is equipped with a feed flow meter (9).
8. The high-efficiency dimethyl sulfide removal device for tebuconazole intermediate epoxy according to claim 1, characterized in that, The thin-film evaporator (3), receiving tank 1 (4), condenser (5) and receiving tank 2 (6) can be provided in two sets, and the feed pipe (7) is provided with a three-way valve that is connected to the two sets of evaporation components respectively.