Production system of oxygen-fluorine cyclization ester

Abstract

The invention discloses an oxygen-fluorine cyclization ester production system, and relates to the technical field of oxygen-fluorine cyclization ester production, the oxygen-fluorine cyclization ester production system comprises a reaction kettle A and a reaction kettle B, the reaction kettle A and the reaction kettle B are connected with a reactor A; the reactor A is connected with a reactor B, and the reactor B is connected with a storage tank A; the reactor B is connected with a centrifugal part, the centrifugal part is connected with a storage tank C, the centrifugal part is connected with a film feeding tank and an extraction heavy component tank, the film feeding tank is connected with an evaporator, and the evaporator is connected with a film receiving tank and a temporary storage tank C; a pump D is connected between the temporary storage tank C and the reaction kettle A, the film receiving tank is connected with a pump E, the pump E is connected with a plug flow kettle, the plug flow kettle is connected with a reduced pressure distillation kettle, and the reduced pressure distillation kettle is connected with a finished product receiving tank; the full-chain continuous automatic production from raw material treatment to final product can be realized, the production efficiency is improved, the energy consumption is reduced, and the stability of the product quality and the safety of operators are ensured.

Description

Technical Field

[0001] The invention relates to the technical field of oxyfluorocyclic ester production, in particular to a production system of oxyfluorocyclic ester. Background Art

[0002] As a key raw material for the synthesis of important pharmaceutical intermediates such as levofloxacin, oxyfluorocyclic esters occupy an important position in the fluorine chemical industry. Traditional production methods generally use kettle-type intermittent reactors. This process requires strict control of reaction conditions, including temperature, pressure, material ratio, etc., to ensure product quality and yield. However, the intermittent operation mode has obvious limitations, such as high workload, cumbersome and complicated procedures, and frequent manual intervention, including material input, reaction control, product unloading, and equipment cleaning. It not only consumes a lot of manpower and material resources, but may also cause fluctuations in product quality between batches, affecting production efficiency and cost control. At the same time, the raw materials used to produce oxyfluorocyclic esters are toxic, and manual operation can easily affect the health of operators.

[0003] In view of the above problems, the present invention proposes an innovative continuous automated oxygen-fluorine series production system, which aims to achieve the transition from intermittent production mode to continuous production mode through technological innovation, and fundamentally improve production efficiency and product quality stability. Summary of the invention

[0004] The purpose of the present invention is to provide a production system of oxyfluorocyclic ester, which realizes continuous automated production of the entire chain from raw material processing to final products by integrating key components such as a dynamic tubular reactor, a conveying unit, and an intelligent control system, thereby improving production efficiency, reducing energy consumption, and ensuring the stability of product quality and the safety of operators.

[0005] The above-mentioned optimized structure of the present invention is realized by the following technical scheme: a production system of oxyfluorocyclic ester, comprising a reactor A and a reactor B, wherein the reactor A is connected to a conveying unit A, the reactor B is connected to a conveying unit B, and the conveying unit A and the conveying unit B are both connected to a reactor A; The discharge port of the reactor A is connected to a filter press A, the filter press A is connected to a temporary storage tank A, the temporary storage tank A is connected to a pump A, the pump A is connected to a reactor B, the feed port of the reactor B is connected to a conveying unit C, and the conveying unit C is connected to a storage tank A; The discharge port of the reactor B is connected to a temporary storage tank B, the feed port of the temporary storage tank B is connected to a conveying unit D, and the conveying unit D is connected to a storage tank B; The temporary storage tank B is connected to a pump F, the pump F is connected to a centrifugal element, the feed port of the centrifugal element is connected to a pump B, the pump B is connected to a storage tank C, the discharge port of the centrifugal element is respectively connected to a film feed tank and an extraction heavy component tank, the film feed tank is connected to a pump C, the pump C is connected to an evaporator, and the discharge port of the evaporator is respectively connected to a film receiving tank and a temporary storage tank C; A pump D is connected between the temporary storage tank C and the reactor A, the film receiving tank is connected to a pump E, the pump E is connected to a plug flow reactor, the plug flow reactor is connected to a vacuum distillation reactor, and the vacuum distillation reactor is connected to a finished product receiving tank.

[0006] In some embodiments, the pump A and the delivery unit C are both connected to a mixer, and a precooler A is connected between the mixer and the reactor B.

[0007] In some embodiments, the conveying unit D and the discharge port of the reactor B are both connected to the precooler B, and the discharge port of the precooler B is connected to the feed port of the temporary storage tank B.

[0008] In some embodiments, the delivery unit A, the delivery unit B, the delivery unit C and the delivery unit D include a filter, a three-head metering pump, a back pressure valve, a regulating valve, a pressure transmitter and a mass flow meter connected in sequence.

[0009] In some embodiments, the feed port of the plug flow kettle is connected to an automatic solid feeder, and a gas delivery pipe is connected between the automatic solid feeder and the plug flow kettle.

[0010] In some embodiments, the centrifugal member includes a plurality of centrifuges connected in series, the centrifuge includes a housing, a vortex disk, a baffle plate, and a drum, at least two hybrid units are provided on the inner wall of the drum, and the hybrid unit is provided between the baffle plate and the vortex disk; The hybrid unit comprises a fixed shaft, one end of which is vertically fixed to the inner wall of the drum, and the other end of which is sleeved with a blade, the blade can rotate on the fixed shaft, and a plurality of through holes are arranged on the blade.

[0011] In some embodiments, a metering tank is connected between the reactor A and the conveying unit A, and the conveying unit B, and a thermometer is provided between the metering tank and the reactor A, and between the reactor A and the filter press A.

[0012] In some embodiments, the reactor A is connected to three storage tanks D, and the three storage tanks D contain toluene, monoester, and triethylamine, respectively.

[0013] In some embodiments, the reactor B contains tetrafluorobenzoyl chloride, the storage tank A contains aminopropanol, the storage tank B contains dilute hydrochloric acid, the storage tank C contains water, and the plug flow reactor is provided with NN-dimethylethylenediamine and potassium fluoride.

[0014] In some embodiments, a control system is also included, and the control system is electrically connected to the conveying unit A, the conveying unit B, the pump A, the conveying unit C, the conveying unit D, the pump B, the pump C, the pump D, the pump E, and the pump F.

[0015] One or more of the above technical solutions in the embodiments of the present invention have at least the following technical effects or advantages: Through the arrangement of reactors, storage tanks, temporary storage tanks, centrifugal parts, evaporators, conveying units, pumps and other structures, the continuous input of raw materials, reaction and continuous output of products can be achieved, the downtime caused by intermittent operation can be eliminated, the production cycle can be shortened and the production efficiency can be improved; the control system can automatically monitor the reaction parameters (such as temperature, flow rate, etc.), accurately adjust the reaction conditions, reduce human errors, improve the quality of finished products, and ensure the consistency of product quality between batches; at the same time, it can reduce manual operation links, protect the safety of operators, reduce manual intervention, reduce energy consumption and improve the utilization rate of raw materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, 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.

[0017] Figure 1 This is a schematic diagram of the production structure of the secondary products of the present invention; Figure 2 It is a structural schematic diagram of the continuous extraction process of the present invention; Figure 3 It is a structural schematic diagram of the evaporation process of the present invention; Figure 4 It is a cross-sectional schematic diagram of the centrifuge of the present invention; Figure 5 For the present invention Figure 4 A magnified schematic diagram of center A.

[0018] In the figure: 1, reactor A; 2, reactor B; 3, reactor A; 4, temporary storage tank A; 5, reactor B; 6, storage tank A; 7, filter press A; 8, temporary storage tank B; 9, storage tank B; 10, centrifugal element; 101, housing; 102, vortex disk; 103, baffle; 104, drum; 105, fixed shaft; 106, paddle; 11, storage tank C; 12, film feed tank; 13, extraction heavy component tank; 14, Evaporator; 15. Plug flow kettle; 16. Conveying unit A; 17. Conveying unit B; 18. Pump A; 19. Conveying unit C; 20. Conveying unit D; 21. Pump B; 22. Pump C; 23. Film receiving tank; 24. Temporary storage tank C; 25. Pump D; 26. Pump E; 27. Mixer; 28. Precooler A; 29. ​​Precooler B; 30. Solid automatic feeder; 31. Metering tank; 32. Pump F; 33. Transfer tank. DETAILED DESCRIPTION

[0019] Embodiments of the present invention are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present invention, and should not be construed as limiting the present invention.

[0020] In the description of the present invention, it should be understood that the terms "length", "width", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship are based on the orientation or position relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0021] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0022] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like 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 a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0023] refer to Figure 1-3 A production system of oxyfluorocyclic esters includes a reactor A1 and a reactor B2. The reactors A1 and B2 can be made of corrosion-resistant materials and have built-in stirring devices for uniformly mixing the initial reaction raw materials. The reactor A1 can be connected to three storage tanks D. The three storage tanks D respectively store toluene, monoester and triethylamine, which are used as the initial reaction raw materials in the production process of oxyfluorocyclic esters. They are uniformly mixed in the reactor A1 to prepare for the subsequent initial reaction. The reactor B2 contains tetrafluorobenzoyl chloride. The reactor A1 is connected to a conveying unit A16 for accurately conveying the raw materials in the reactor A1. The reactor B2 is connected to a conveying unit B17 for accurately conveying the raw materials in the reactor B2. The conveying units A16 and B17 are both connected to a reactor A3. The reactor A3 can adopt an efficient heat exchange design to maintain a suitable reaction temperature, so that the raw materials in the reactor A1 and the raw materials in the reactor B2 are mixed, a primary reaction occurs, and a primary product is obtained.

[0024] The discharge port of reactor A3 is connected with filter press A7, which may be a bag filter for filtering the primary product. Filter press A7 is connected with temporary storage tank A4 for storing the primary product. Temporary storage tank A4 is connected with pump A18, which is connected with reactor B5. Reactor B5 may be a dynamic tubular reactor, and the ear holes are designed with high-efficiency heat exchange to maintain a suitable reaction temperature. The primary product in temporary storage tank A4 can be transported to reactor B5 through pump A18. The feed port of reactor B5 is connected with conveying unit C19, which is connected with storage tank A6. Raw materials for secondary reactions, such as aminopropanol, are stored in storage tank A6. The raw materials for secondary reactions are accurately transported to storage tank A6 through conveying unit C19. The cooperation of pump A18 and conveying unit C19 realizes continuous transportation and precise control of reactants in reactor B5.

[0025] The discharge port of the reactor B5 is connected to a temporary storage tank B8 for storing secondary products. The feed port of the temporary storage tank B8 is connected to a conveying unit D20. The conveying unit D20 is connected to a storage tank B9. The storage tank B9 can store acidic substances such as dilute hydrochloric acid. The conveying unit D20 can accurately control the acidic substances delivered to the temporary storage tank B8 to adjust the pH value in the temporary storage tank B8.

[0026] The temporary storage tank B8 is connected to a pump F32, which is connected to a centrifugal element 10. The centrifugal element 10 is used to separate the mixture in the temporary storage tank B8. The feed port of the centrifugal element 10 is connected to a pump B21, which is connected to a storage tank C11. The storage tank C11 can store water and other washing materials for washing the mixture in the temporary storage tank B8; the discharge port of the centrifugal element 10 is respectively connected to a film feed tank 12 and an extraction heavy component tank 13. The film feed tank 12 is used to receive the separated material, and the extraction heavy component tank 13 is used to receive and store the separated wastewater, which is convenient for subsequent wastewater treatment. The film feed tank 12 is connected to a pump C22, which is connected to an evaporator 14. The evaporator 14 can adopt a multi-effect evaporation technology to reduce energy consumption. The pump C22 can continuously feed into the evaporator 14 to evaporate and separate the substances in the separation. The discharge port of the evaporator 14 is respectively connected to a film receiving tank 23 and a temporary storage tank C24. The film receiving tank 23 is used to receive the purified material after evaporation, and the temporary storage tank C24 is used to store the evaporated material. A condenser can be connected between the temporary storage tank C24 and the evaporator 14 to cool the evaporated material, so that it can be quickly liquefied and the continuity of production can be accelerated.

[0027] In some embodiments, the centrifugal element 10 includes multiple centrifuges, and the multiple centrifuges are connected in series by connecting the light phase outlet of one centrifuge to the light phase inlet of another centrifuge, and connecting the heavy phase outlet of one centrifuge to the heavy phase inlet of another centrifuge, thereby performing multiple separations of the mixture entering the centrifugal element 10 and improving the separation efficiency.

[0028] refer to Figure 4-5 The centrifuge includes a housing 101, a vortex disk 102, a light phase inlet, a heavy phase inlet, a light phase outlet, a heavy phase outlet, a baffle 103, a drum 104, a heavy phase weir plate, and a light phase weir plate. At least two hybrid units are arranged on the inner wall of the drum 104, and the hybrid unit is arranged between the baffle 103 and the vortex disk 102. The hybrid unit includes a fixed shaft 105, one end of the fixed shaft 105 is vertically fixed on the inner wall of the drum 104, and the other end is sleeved with a blade 106. The blade 106 can be an airfoil with a large frontal area or a propeller-like blade to maximize the contact area with the mixed liquid and generate sufficient shear force and driving force; the blade 106 can rotate on the fixed shaft 105, and a plurality of through holes are arranged on the blade 106, which can allow part of the mixed liquid to pass through, so that the mixed liquid pushes the blade 106 to rotate, while reducing the resistance of the blade 106 to the flow of the mixed liquid, avoiding the influence of the blade 106 on the later separation of the mixed liquid.

[0029] The light phase liquid flows in from the light phase inlet, and the heavy phase liquid flows in from the heavy phase inlet. The two liquids converge above the vortex disk 102 to form a mixed liquid, and flow into the drum 104. Due to the natural stratification characteristics of the fluid and the effect of the vortex disk 102, the mixed liquid begins to form preliminary turbulence. As the mixed liquid continues to flow into the drum 104, they collide and interact with the rotating blades 106. The paddle 106 is rotated on the fixed shaft 105. The rotating paddle 106 applies a lateral shear force to the liquid on the one hand, and an upward driving force to the liquid on the other hand, which can increase the contact area between the drum 104 and the mixed liquid, so that the mixed liquid moves toward the inner wall of the drum 104 under the action of centrifugal force and is stirred and mixed by the paddle 106, thereby improving the mixing efficiency of the two liquids in the mixed liquid. At the same time, the mixed liquid impacts the paddle 106, and the friction and collision between the paddle 106 will cause heat between the paddle 106 and the mixed liquid, resulting in a gradual increase in the temperature of the mixed liquid. The increase in temperature can enhance the activity of the molecules of the light phase liquid and the heavy phase liquid, reduce the viscosity of the liquid, and further improve the mixing efficiency of the two liquids. At the same time, the dissolution and cleaning speed between the light phase liquid and the heavy phase liquid is increased, thereby improving the separation effect of the mixed liquid in the later stage.

[0030] Under the action of centrifugal force, the light phase and the heavy phase in the mixed liquid begin to gradually separate and move toward the inner wall of the drum 104. In this process, the rotation and stirring action of the blades 106 help to accelerate the stratification process and reduce the residual impurities in the mixed liquid.

[0031] A plurality of blades 106 are arranged at intervals along a spiral ascending curve on the inner wall of the drum 104. The plurality of blades 106 rotate simultaneously to form a spiral ascending flow channel on the inner wall of the drum 104, so that the mixed liquid in the drum 104 can rise along the flow channel, thereby increasing the rising speed of the mixed liquid, and at the same time, the mixed liquid is subjected to continuous shearing and stirring, thereby improving the separation efficiency.

[0032] An annular groove is provided on the fixed shaft 105, and the paddle 106 is sleeved in the annular groove. The height of the annular groove is greater than the thickness of the connection between the paddle 106 and the fixed shaft 105, so that the paddle 106 has a certain sliding space on the fixed shaft 105, which can produce slight sliding and swinging, thereby further enhancing the turbulence effect of the paddle 106 on the mixed liquid.

[0033] A pump D25 is connected between the temporary storage tank C24 and the reactor A1, and the liquefied evaporated material is transported to the reactor A1 through the pump D25 to serve as the initial reaction raw material, thereby realizing partial recycling of the raw material, reducing the loss and waste of the material, and thus reducing the input cost of the material; the film receiving tank 23 is connected to a pump E26, and the pump E26 is connected to a plug flow kettle 15, in which NN-dimethylethylenediamine and potassium fluoride are arranged, and the plug flow kettle 15 is connected to a vacuum distillation kettle, and the product in the film receiving tank 23 is transported to the plug flow kettle 15 and the vacuum distillation kettle through the pump E26 to complete the final refining to obtain high-purity oxyfluorocyclic ester, and the vacuum distillation kettle is connected to a finished product receiving tank for storing the final oxyfluorocyclic ester product produced.

[0034] In some embodiments, there may be multiple plug flow kettles 15, and a transfer tank 33 may be connected between the film receiving tank 23 and the plug flow kettle 15, so as to avoid interference between the product collection process and the transportation process in the film receiving tank 23, thereby realizing simultaneous collection and transportation of the product in the film receiving tank 23.

[0035] In some embodiments, pump A18 and conveying unit C19 are connected to mixer 27 to improve the mixing uniformity between materials and facilitate sufficient reaction in the later stage. A precooler A28 is connected between mixer 27 and reactor B5. Precooler A28 can adopt a high-efficiency fin structure to accelerate cooling. It can cool the material conveyed from mixer 27 to reactor B5 to reach a temperature suitable for reaction to achieve a good reaction. The cooling medium of precooler A28 can adopt ethylene glycol, which can increase the cooling speed and speed up production.

[0036] In some embodiments, the conveying unit D20 and the discharge port of the reactor B5 are both connected to the precooler B29. The precooler B29 can adopt a high-efficiency fin structure to accelerate cooling. The discharge port of the precooler B29 is connected to the feed port of the temporary storage tank B8, and the material after the reaction of the reactor B5 and the material in the storage tank B9 can be cooled to keep them at a suitable temperature, thereby avoiding excessively high temperature during the pH adjustment process, which causes reactions between the substances and affects the pH of the substances after mixing.

[0037] In some embodiments, the delivery unit A16, the delivery unit B17, the delivery unit C19 and the delivery unit D20 include a filter, a three-head metering pump, a back pressure valve, a regulating valve, a pressure transmitter and a mass flow meter connected in sequence, which can filter and deliver the raw materials required for the reaction, and realize precise control of the raw material flow, thereby realizing precise control of the reaction. The built-in filter and the three-head metering pump ensure the purity and metering accuracy of the raw materials, the back pressure valve and the regulating valve maintain a stable delivery pressure and flow, and the pressure transmitter and the mass flow meter monitor in real time and feedback data to the control system.

[0038] In some embodiments, the feed port of the plug flow kettle 15 is connected to a solid automatic feeder 30, which can be used to add solid reaction raw material potassium fluoride into the plug flow kettle 15. A gas delivery pipe is connected between the solid automatic feeder 30 and the plug flow kettle 15. Nitrogen is provided in the gas delivery pipe to provide a nitrogen protective atmosphere to prevent the mixture in the plug flow kettle 15 from contacting with air during the reaction, thereby affecting the purity of the oxyfluorocyclic ester generated after the reaction; at the same time, it can be used for positive pressure gas replenishment when the solid automatic feeder 30 delivers potassium fluoride to prevent the solid feeding port from being blocked.

[0039] In some embodiments, a metering tank 31 is connected between the reactor A3 and the delivery unit A16 and the delivery unit B17, which can quantitatively deliver the amount of raw materials into the reactor A3 and compare it with the data of the three-head metering pumps in the delivery unit A16 and the delivery unit B17, so as to facilitate data analysis of the delivery process and subsequent processing; thermometers are provided between the metering tank 31 and the reactor A3, and between the reactor A3 and the filter press A7, which can detect important temperature data in the reaction process, so that the reaction process is always within the set temperature range, and achieve better reaction effect.

[0040] In some embodiments, a control system is also included. The control system is electrically connected to conveying unit A16, conveying unit B17, pump A18, conveying unit C19, conveying unit D20, pump B21, pump C22, pump D25, pump E26, and pump F32. A DCS operating system can be used to achieve unified management, ensure that each unit works accurately and collaboratively, and realize automation and intelligent regulation of the production process, thereby achieving efficient, safe, reliable, and intelligent management of the production process.

[0041] In some embodiments, each reactor, storage tank, temporary storage tank, delivery unit, pump and precooler may be provided with a thermometer electrically connected to the control system, and the operating status of each key point can be monitored in real time by the thermometer. The data is processed and fed back to the central processor to achieve precise control of the delivery unit, pump, reactor and other equipment. For example, when the reaction temperature deviates from the set value, the system will automatically adjust the flow rate of the cooling medium in the corresponding precooler to maintain the stability of the reaction conditions. At the same time, it can support remote monitoring and fault warning to improve the safety and flexibility of production.

[0042] Embodiment 1: First, toluene, monoester, triethylamine and other raw materials are premixed in proportion and added to the reactor A1. In this embodiment, 1000L toluene, 800L monoester and 200L triethylamine are used. Preliminary mixing is performed under appropriate conditions through precise temperature control and stirring, and the mixture is preheated to an appropriate temperature under stirring. At the same time, 200L tetrafluorobenzoyl chloride is added to the reactor B2 and stirred to an appropriate temperature; the conveying unit A16 conveys the mixed solution formed by toluene, monoester and triethylamine into the reactor A3, and the conveying unit B17 conveys the tetrafluorobenzoyl chloride into the reactor A3 and mixes with the mixed solution to produce a preliminary reaction; in this process, the metering tank 31 is used to accurately control the raw material feeding amount, and the thermometer monitors the temperature of the reaction solution to ensure that the reaction conditions are stable, and the corresponding parameters are fed back to the control system.

[0043] The mixed solution and tetrafluorobenzoyl chloride are continuously catalytically converted in the reactor A3, and the reactor A3 can maintain a constant temperature of 200° C. for 2 hours to generate a primary product (tetrafluoroanisole solution). The tetrafluoroanisole solution is then sent to the filter press A7 to remove insoluble matter to obtain a pure reaction liquid, and then enters the temporary storage tank A4 for temporary storage. The temperature of the pure reaction liquid in the temporary storage tank A4 is controlled at room temperature and waits for the next step of processing.

[0044] Storage tank A6 is loaded with 500L of aminopropanol, which is accurately transported by conveying unit C19 and then mixed with the pure reaction liquid in temporary storage tank A4 and sent to reactor B5. Before entering reactor B5, aminopropanol and pure reaction liquid are fully mixed in mixer 27, and the temperature of the mixed liquid of aminopropanol and pure reaction liquid is reduced to a condition suitable for secondary reaction by precooler A28 to ensure the optimization of reaction conditions.

[0045] After aminopropanol and pure reaction liquid are fully reacted in reactor B5, an oxyfluorocyclic ester intermediate material is obtained. The oxyfluorocyclic ester intermediate material can be filtered through a filter press to obtain a toluene mixed liquid, which can pass through a mass flow meter and enter the precooler B29 for cooling. At the same time, an appropriate amount of dilute hydrochloric acid from the storage tank B9 is input into the precooler B29 for cooling through the conveying unit D20, and mixed with the toluene mixed liquid in the temporary storage tank B8 to adjust the pH value of the toluene mixed liquid to the desired range.

[0046] Through the control system, the feed rates of pumps B21 and F32 are set, and the mixture in the temporary storage tank B8 and the water in the storage tank C11 are continuously transported to the two feed ports of the centrifugal element 10, so that the mixture and the water are fully mixed and separated in the centrifugal element 10, and the separated clean liquid phase enters the membrane feed tank 12, and the separated impurities are mixed with water and flow to the extraction heavy component tank 13, which is convenient for the subsequent treatment and utilization of the wastewater.

[0047] The feed rate of pump C22 is set so that the separated clean liquid phase is sent to evaporator 14, evaporated and concentrated under reduced pressure conditions to obtain toluene vapor and amination liquid. The toluene vapor is cooled and liquefied by the condenser, flows into the temporary storage tank C24, and is sent back to the reactor A1 through pump D25 to achieve the recycling of raw materials; the amination liquid flows into the film receiving tank 23.

[0048] A set amount of NN-dimethylethylenediamine and potassium fluoride are delivered to the plug flow kettle 15. Potassium fluoride can be added through the solid automatic feeder 30, and the plug flow kettle 15 is connected to the nitrogen delivery pipe so that the plug flow kettle 15 is in a nitrogen atmosphere and isolated from the air. The feed amount of the pump E26 is set, and the amination liquid is continuously delivered to the plug flow kettle 15. At the same time, the stirring device in the plug flow kettle 15 stirs to increase the reaction speed. The substances that have reacted completely in the plug flow kettle 15 are connected to the filter press for filtration, and the filtrate is then sent to the vacuum distillation kettle. The final purification is completed by evaporation to a small volume of discharge centrifugation to obtain high-purity oxyfluoride cyclic ester, and the final product is sent to the finished product receiving tank.

[0049] During the entire production process, the control system continuously monitors the temperature, pressure, flow and other parameters of each key point, and automatically adjusts the working status of the conveying unit, pump and reactor through preset algorithms to ensure the stability and safety of the reaction conditions.

[0050] The use of the solid automatic feeder 30, combined with the nitrogen-protected gas delivery pipe, effectively controls the uniform addition of solid materials, avoids the intervention of oxygen, and improves the safety and efficiency of the chemical reaction.

[0051] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some of the technical features may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A production system of oxyfluorocyclic ester, characterized in that: The invention comprises a reactor A (1) and a reactor B (2), wherein the reactor A (1) is connected to a conveying unit A (16), the reactor B (2) is connected to a conveying unit B (17), and the conveying unit A (16) and the conveying unit B (17) are both connected to a reactor A (3); The discharge port of the reactor A (3) is connected to a filter press A (7), the filter press A (7) is connected to a temporary storage tank A (4), the temporary storage tank A (4) is connected to a pump A (18), the pump A (18) is connected to a reactor B (5), the feed port of the reactor B (5) is connected to a conveying unit C (19), and the conveying unit C (19) is connected to a storage tank A (6); The discharge port of the reactor B (5) is connected to a temporary storage tank B (8), the feed port of the temporary storage tank B (8) is connected to a conveying unit D (20), and the conveying unit D (20) is connected to a storage tank B (9); The temporary storage tank B (8) is connected to a pump F (32), the pump F (32) is connected to a centrifugal element (10), the feed port of the centrifugal element (10) is connected to a pump B (21), the pump B (21) is connected to a storage tank C (11), the discharge port of the centrifugal element (10) is respectively connected to a film feed tank (12) and an extraction heavy component tank (13), the film feed tank (12) is connected to a pump C (22), the pump C (22) is connected to an evaporator (14), and the discharge port of the evaporator (14) is respectively connected to a film receiving tank (23) and a temporary storage tank C (24); A pump D (25) is connected between the temporary storage tank C (24) and the reactor A (1), the film receiving tank (23) is connected to a pump E (26), the pump E (26) is connected to a plug flow reactor (15), the plug flow reactor (15) is connected to a vacuum distillation reactor, and the vacuum distillation reactor is connected to a finished product receiving tank.

2. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The pump A (18) and the conveying unit C (19) are both connected to a mixer (27), and a precooler A (28) is connected between the mixer (27) and the reactor B (5).

3. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The conveying unit D (20) and the discharge port of the reactor B (5) are both connected to the precooler B (29), and the discharge port of the precooler B (29) is connected to the feed port of the temporary storage tank B (8).

4. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The conveying unit A (16), the conveying unit B (17), the conveying unit C (19) and the conveying unit D (20) include a filter, a three-head metering pump, a back pressure valve, a regulating valve, a pressure transmitter and a mass flow meter which are connected in sequence.

5. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The feed inlet of the plug flow kettle (15) is connected to an automatic solid feeder (30), and a gas delivery pipe is connected between the automatic solid feeder (30) and the plug flow kettle (15).

6. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The centrifugal element (10) comprises a plurality of centrifuges connected in series, the centrifuge comprising a housing (101), a vortex disk (102), a baffle plate (103), and a rotating drum (104); at least two hybrid units are provided on the inner wall of the rotating drum (104); the hybrid units are provided between the baffle plate (103) and the vortex disk (102); The hybrid unit comprises a fixed shaft (105), one end of the fixed shaft (105) is vertically fixed to the inner wall of the drum (104), and the other end is sleeved with a paddle (106), the paddle (106) can rotate on the fixed shaft (105), and the paddle (106) is provided with a plurality of through holes.

7. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: A metering tank (31) is connected between the reactor A (3) and the conveying unit A (16) and the conveying unit B (17), and a thermometer is provided between the metering tank (31) and the reactor A (3), and between the reactor A (3) and the filter press A (7).

8. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The reactor A (1) is connected to three storage tanks D, in which toluene, monoester and triethylamine are stored respectively.

9. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The reaction kettle B (2) contains tetrafluorobenzoyl chloride, the storage tank A (6) contains aminopropanol, the storage tank B (9) contains dilute hydrochloric acid, the storage tank C (11) contains water, and the plug flow kettle (15) contains NN-dimethylethylenediamine and potassium fluoride.

10. The production system of an oxyfluorocyclic ester according to claim 1, characterized in that: The invention also includes a control system, which is electrically connected to the conveying unit A (16), the conveying unit B (17), the pump A (18), the conveying unit C (19), the conveying unit D (20), the pump B (21), the pump C (22), the pump D (25), the pump E (26), and the pump F (32).

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