Modular organic electrochemical fluorination electrolysis system
Patent Information
- Application Number
- CN202611011778.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-07-08
- Publication Date
- 2026-10-16
AI Technical Summary
[0005]针对现有技术的不足,本发明提供一种模块化有机物电化学氟化电解系统,通过模块化拆分与集成设计,实现电解单元的灵活组合与扩容,优化电解液循环、气液分离及温控体系,配合智能化控制系统,提升电解效率、运行稳定性与安全性能,解决传统系统规模化适配差、效率低、安全性弱、运维难的技术难题
1)模块化灵活适配:采用可独立拆装的电解模块设计,可根据生产产能灵活增减模块数量,适配大型规模化生产,占地面积小,管路与电路布局简洁,便于设备安装与扩容;
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Figure CN122918588A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of electrochemical fluorination technology, specifically relating to a modular organic electrochemical fluorination electrolysis system. Background Technology
[0002] Electrochemical fluorination is one of the core technologies for preparing fluorinated organic compounds. Compared with chemical fluorination, it has advantages such as mild reaction conditions, high fluorination selectivity, excellent product purity, and no need to use highly toxic fluorinating reagents. It has been widely used in the industrial production of products such as perfluorosulfonyl fluoride, perfluoroalkanes, perfluoroethers, fluorinated surfactants, and fluorinated pharmaceutical intermediates.
[0003] Existing electrochemical fluorination electrolysis systems for organic compounds generally suffer from the following technical defects: 1) Poor adaptability to large-scale production: Traditional electrolysis systems are mostly integrated fixed structures with limited processing capacity of a single set of equipment. They cannot be flexibly expanded according to production needs. In large-scale production scenarios, multiple independent sets of equipment need to be connected in parallel, resulting in a large footprint, complex pipeline layout, and extremely high maintenance difficulty. 2) Insufficient electrolysis efficiency and stability: unreasonable electrode arrangement, poor electrolyte circulation, uneven temperature and concentration distribution during the reaction process, which can easily lead to problems such as local overheating, increased side reactions, and decreased current efficiency. Moreover, electrode replacement and system maintenance require a complete shutdown, which seriously affects continuous production efficiency. 3) Weak safety performance: The electrochemical fluorination process uses anhydrous hydrofluoric acid as the main electrolyte, which is highly corrosive and toxic. The reaction produces hydrogen and fluoride gases. Traditional systems have poor gas-liquid separation, which can easily lead to gas mixing and electrolyte leakage risks. There is a lack of a complete intelligent safety monitoring and emergency control mechanism. 4) Low maintenance and versatility: The system has a high degree of integration among its components. Failure of a single component can easily lead to the paralysis of the entire system. Replacement of components requires customized processing, resulting in poor versatility, high maintenance costs, and long cycles, making it difficult to meet the needs of continuous and large-scale industrial production.
[0004] Therefore, developing a modular organic electrochemical fluorination electrolysis system that is flexibly expandable, highly efficient, safe and controllable, and easy to operate and maintain has become an urgent technical problem to be solved in this field. Summary of the Invention
[0005] To address the shortcomings of existing technologies, this invention provides a modular organic electrochemical fluorination electrolysis system. Through modular disassembly and integration design, it enables flexible combination and expansion of electrolysis units, optimizes electrolyte circulation, gas-liquid separation and temperature control systems, and, in conjunction with an intelligent control system, improves electrolysis efficiency, operational stability and safety performance. This solves the technical problems of poor large-scale adaptability, low efficiency, weak safety and difficult operation and maintenance of traditional systems.
[0006] To achieve the above objectives, the present invention adopts the following technical solution: A modular organic electrochemical fluorination electrolysis system includes a modular electrolysis unit, an electrolyte circulation supply unit, a gas-liquid separation and recovery unit, a temperature control unit, and a control unit; The modular electrolysis unit is composed of several independent electrolysis modules connected in series or parallel. Each group of electrolysis modules has the same structure and can be independently disassembled and operated. The electrolyte circulation supply unit, gas-liquid separation and recovery unit, and temperature control unit are respectively connected to the modular electrolysis unit. The control unit is electrically connected to the modular electrolysis unit, the electrolyte circulation supply unit, the gas-liquid separation and recovery unit, and the temperature control unit, respectively.
[0007] Preferably, the modular electrolysis unit includes multiple electrolysis modules, each adopting a pressure filter type single-pole parallel structure, and each electrolysis module is provided with an inlet and an outlet.
[0008] Preferably, multiple electrolysis modules are connected to each other via a positive conductive bus and a negative conductive bus. The positive conductive bus is connected to the anode of the electrolysis module, and the negative conductive bus is connected to the cathode of the electrolysis module. The other end of the positive conductive bus is connected to the positive terminal of the power supply cabinet, and the other end of the negative conductive bus is connected to the negative terminal of the power supply cabinet.
[0009] The electrolysis module adopts a pressure filter type single-pole parallel structure, including a module shell, anode assembly, cathode assembly, ion conduction diaphragm, and sealing gasket. The module shell is made of PVDF or PFA fluoroplastic material resistant to hydrofluoric acid corrosion, and has an independent electrolysis reaction chamber inside. The anode assembly uses nickel-based alloy electrodes, and the cathode assembly uses stainless steel electrodes. The electrode surfaces are opened with uniformly distributed guide grooves. The ion conduction diaphragm is placed between the anode and cathode to isolate the anode and cathode areas and prevent gas mixing.
[0010] Power cabinet: It is a detachable steel structure used to fix each group of electrolysis modules. The modules are connected to each other through sealed connectors to achieve quick connection of pipelines and circuits. The conductive busbars are connected to the anode and cathode of each group of electrolysis modules to achieve unified power supply or independent power supply for each zone.
[0011] Each electrolysis module is equipped with an independent inlet, outlet, and exhaust port, allowing for independent electrolyte circulation and gas-liquid discharge. In case of a single module failure, it can be shut down for maintenance without affecting the operation of other modules.
[0012] Preferably, the electrolyte circulation supply unit includes an electrolyte storage tank with a feed port and a level sensor. The electrolyte storage tank is made of corrosion-resistant material and stores a mixture of anhydrous hydrofluoric acid and organic raw materials as an electrolyte. The tank is equipped with a level sensor and a feed port to achieve automatic electrolyte replenishment.
[0013] Preferably, the electrolyte circulation supply unit further includes a magnetically driven corrosion-resistant circulation pump, a filter, and a branch supply pipe that are sequentially connected to the electrolyte storage tank. The branch supply pipe is connected to each group of electrolysis modules respectively, and a flow sensor and a flow regulating valve are installed on the pipeline connecting the branch supply pipe and the electrolysis module.
[0014] A magnetically driven, corrosion-resistant circulating pump prevents pump body leakage. The main supply pipe connects to the electrolyte storage tank, and branch supply pipes connect to the inlets of each electrolysis module. Flow regulating valves are located on the branch supply pipes. An intelligent control unit independently adjusts the electrolyte flow rate of each module based on electrolysis reaction parameters to ensure uniform electrolyte supply. A filter is installed on the main supply pipe to filter impurities in the electrolyte, prevent electrode clogging, and extend electrode life.
[0015] Preferably, the gas-liquid separation and recovery unit includes a gas-liquid separator. The upper end of the gas-liquid separator is connected to a gas condenser, and the lower end of the gas-liquid separator is connected to a liquid phase reflux pipe, which is connected to an electrolyte storage tank. The gas-liquid separator is configured with the outlet and exhaust port corresponding to each electrolysis module, and adopts a multi-stage separation structure to achieve rapid gas-liquid separation of electrolysis products. The liquid phase electrolyte is returned to the electrolyte storage tank through the liquid phase reflux pipe for recycling. The gas condenser is connected to the gas phase outlet of the gas-liquid separator to condense and reflux the hydrofluoric acid vapor entrained in the gas, reducing raw material loss. The condensed target fluorine-containing gas is transported to the subsequent refining process, and the by-product hydrogen is purified by the tail gas treatment component before being discharged in compliance with standards.
[0016] Preferably, the gas-liquid separator is equipped with a pressure sensor and a liquid level monitoring sensor. This allows for real-time monitoring of the pressure and liquid level in the separation chamber, preventing gas-liquid cross-contamination.
[0017] Preferably, the temperature control unit includes an inlet heat exchanger and an outlet heat exchanger. The inlet heat exchanger is located on the pipeline between the electrolyte storage tank and the magnetically driven anti-corrosion circulating pump. One end of the outlet heat exchanger is connected to the inlet of the gas-liquid separator, and the other end of the outlet heat exchanger is connected to the electrolysis module.
[0018] Preferably, the temperature sensor is electrically connected to the control unit.
[0019] The temperature control unit also includes heat exchange coils and temperature sensors. The heat exchange coils are embedded inside the shells of each electrolysis module and inside the electrolyte storage tank. The cooling medium circulator uses ethylene glycol aqueous solution as the cooling medium, which removes the heat generated by the electrolysis reaction in real time through the heat exchange coils. The temperature sensors are respectively set inside the electrolysis module, the electrolyte storage tank, and the gas-liquid separator. The intelligent control unit adjusts the flow rate of the cooling medium according to the real-time temperature data to stably control the electrolysis reaction temperature within the optimal range of 0-15℃, avoiding side reactions caused by excessive temperature.
[0020] Preferably, the intelligent control unit includes an alarm device, a DCS control cabinet, and a data acquisition module connected in sequence. The data acquisition module is electrically connected to the modular electrolysis unit, the electrolyte circulation supply unit, the gas-liquid separation and recovery unit, and the temperature control unit, respectively, to realize fully automated control of the entire process.
[0021] The data acquisition module collects temperature, pressure, flow rate, liquid level, current, and voltage parameters of each unit in real time and transmits them to the DCS control cabinet. The system sets alarm thresholds for over-temperature, over-pressure, abnormal liquid level, and abnormal current. When an alarm is triggered, emergency control is automatically activated (such as cutting off power supply, stopping liquid supply, and starting emergency exhaust), realizing intelligent and safe operation of the entire process.
[0022] The present invention has the following beneficial effects: 1) Modular and flexible adaptation: It adopts an independently detachable electrolysis module design, which can flexibly increase or decrease the number of modules according to the production capacity, adapting to large-scale production, with a small footprint, simple pipeline and circuit layout, and easy equipment installation and expansion. 2) Significantly improved electrolysis efficiency: The electrode guide channel and independent electrolyte circulation design ensure uniform electrolyte distribution, rapid heat removal from the reaction, precise temperature control, and an increase in current efficiency of more than 20%, reducing side reactions and achieving product purity ≥99.5%; it also improves the uniformity of electrolyte flow and the efficiency of heat exchange, increases current efficiency, and ensures product purity.
[0023] 3) Comprehensive optimization of safety performance: Fully corrosion-resistant and sealed structure, independent gas-liquid separation and intelligent emergency control, eliminating the risk of hydrofluoric acid leakage and gas mixing explosion, and fully automated monitoring to reduce the safety hazards of manual operation; 4) Convenient operation and maintenance and reduced costs: Each module operates independently, and a single fault can be repaired individually without overall shutdown, improving production continuity and reducing operation and maintenance costs; the modules are highly versatile, and parts are easy to replace, reducing operation and maintenance costs by more than 30%. 5) High raw material utilization: The electrolyte is recycled and hydrofluoric acid vapor is condensed and refluxed, reducing raw material loss and meeting the requirements of green production. It is especially suitable for the efficient and stable electrolytic preparation of perfluorinated organic compounds and fluorine-containing fine chemicals for industrial-scale production. Attached Figure Description
[0024] Figure 1 This is a schematic diagram of the overall system structure of the present invention.
[0025] In the diagram, the modular electrolysis unit consists of: 101-electrolysis module, 102-power cabinet, 103-positive electrode conductive busbar, 104-negative electrode conductive busbar, 105-liquid inlet, and 106-liquid outlet. Electrolyte circulation supply unit: 201-Electrolyte storage tank, 202-Circulation pump, 203-Filter, 204-Flow regulating valve, 205-Flow sensor, 206-Branch supply pipe, 207-Level sensor, 208-Feeding port; Gas-liquid separation and recovery unit: 301-Gas-liquid separator, 302-Gas condenser, 303-Liquid phase reflux pipe, 304-Liquid level monitoring sensor, 305-Pressure sensor; Temperature control unit: 401-Inlet heat exchanger, 402-Outlet heat exchanger, 403-Temperature sensor; Intelligent control unit: 501-DCS control cabinet, 502-alarm device, 503-data acquisition module. Detailed Implementation
[0026] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. These embodiments are only used to explain the present invention and are not intended to limit the scope of protection of the present invention.
[0027] Example 1
[0028] A modular organic electrochemical fluorination electrolysis system includes a modular electrolysis unit, an electrolyte circulation supply unit, a gas-liquid separation and recovery unit, a temperature control unit, and a control unit; The modular electrolysis unit is composed of several independent electrolysis modules 101 connected in series or parallel. Each group of electrolysis modules 101 has the same structure and can be independently disassembled and operated. The electrolyte circulation supply unit, gas-liquid separation and recovery unit, and temperature control unit are respectively connected to the modular electrolysis unit. The control unit is electrically connected to the modular electrolysis unit, the electrolyte circulation supply unit, the gas-liquid separation and recovery unit, and the temperature control unit, respectively.
[0029] The modular electrolysis unit includes multiple electrolysis modules 101. Each electrolysis module 101 adopts a pressure filter type single-pole parallel structure. Each electrolysis module 101 is provided with an inlet 105 and an outlet 106.
[0030] Multiple electrolysis modules 101 are connected to each other via a positive conductive bus 103 and a negative conductive bus 104. The positive conductive bus 103 is connected to the anode of the electrolysis module 101, and the negative conductive bus 104 is connected to the cathode of the electrolysis module 101. The other end of the positive conductive bus 103 is connected to the positive terminal of the power supply cabinet 102, and the other end of the negative conductive bus 104 is connected to the negative terminal of the power supply cabinet 102.
[0031] The electrolyte circulation supply unit includes an electrolyte storage tank 201, a feeding port 208 on the electrolyte storage tank 201, and a liquid level sensor 207 on the electrolyte storage tank 201.
[0032] The electrolyte circulation supply unit also includes a magnetically driven anti-corrosion circulation pump 202, a filter 203, and a branch supply pipe 206 that are sequentially connected to the electrolyte storage tank 201. The branch supply pipe 206 is connected to each group of electrolysis modules 101 respectively. A flow sensor 205 and a flow regulating valve 204 are installed on the pipeline connecting the branch supply pipe 206 and the electrolysis module 101.
[0033] The gas-liquid separation and recovery unit includes a gas-liquid separator 301, the upper end of which is connected to a gas condenser 302, and the lower end of which is connected to a liquid phase reflux pipe 303, which is connected to an electrolyte storage tank 201.
[0034] The gas-liquid separator 301 is equipped with a pressure sensor 305 and a liquid level monitoring sensor 304.
[0035] The temperature control unit includes an inlet heat exchanger 401 and an outlet heat exchanger 402. The inlet heat exchanger 401 is located on the pipeline between the electrolyte storage tank 201 and the magnetically driven anti-corrosion circulating pump 202. One end of the outlet heat exchanger 402 is connected to the inlet of the gas-liquid separator 301, and the other end of the outlet heat exchanger 402 is connected to the electrolysis module 101.
[0036] The temperature control unit also includes heat exchange coils and temperature sensors 403; the heat exchange coils are respectively embedded inside the shells of each group of electrolysis modules 101 and inside the electrolyte storage tank 201, and the cooling medium circulator uses ethylene glycol aqueous solution as the cooling medium; the temperature sensors 403 are respectively installed on the pipelines of the electrolysis module 101, the electrolyte storage tank 201 and the gas-liquid separator 301, and the temperature sensors 403 are electrically connected to the control unit 5.
[0037] The intelligent control unit includes an alarm device 502, a DCS control cabinet 501, and a data acquisition module 503 connected in sequence. The data acquisition module 503 is electrically connected to the modular electrolysis unit, the electrolyte circulation supply unit, the gas-liquid separation and recovery unit, and the temperature control unit, respectively.
[0038] Combined with appendix Figure 1 A modular organic electrochemical fluorination electrolysis system includes four independent electrolysis modules 101 forming a modular electrolysis unit; the power supply cabinet 102 adopts an expandable IGBT high-frequency switching structure; and the electrolyte storage tank 201 has a volume of 10m³. 3 Made of PFA perfluorinated material, it stores a mixed electrolyte of anhydrous hydrofluoric acid and octane. The circulating pump 202 is a magnetically driven corrosion-resistant pump with a flow rate of 250 m³ / h. 3 / h, the main liquid supply pipe is connected to the electrolyte storage tank 201, and the four branch liquid supply pipes 206 are respectively connected to the liquid inlets 105 of the four sets of electrolysis modules 101. Each branch liquid supply pipe 206 is equipped with a flow regulating valve 204 to achieve independent flow control; the filter 203 is made of polytetrafluoroethylene with a filtration accuracy of 5μm, and is set at the front end of the circulation pump 202 to filter electrolyte impurities.
[0039] In the gas-liquid separation and recovery unit, the gas-liquid separator 301 adopts a cyclone separation structure. Each electrolysis module 101 corresponds to one gas-liquid separator 301. The gas phase outlet of the gas-liquid separator 301 is connected to the gas condenser 302. The condensation temperature is controlled at -5℃. After the hydrofluoric acid vapor entrained in the gas phase is condensed, it is returned to the electrolyte storage tank 201 through the liquid phase return pipe 303. The target fluorine-containing product gas is transported to the refining process. The gas-liquid separator 301 is equipped with a pressure sensor 305 and a liquid level monitoring sensor 304 to monitor the operating parameters in real time.
[0040] In the temperature control unit, the inlet heat exchanger 401 and the outlet heat exchanger 402 are made of 316 stainless steel. Temperature sensors 403 are respectively installed on the electrolysis module 101, the gas-liquid separator 301, the inlet heat exchanger 401 and the outlet heat exchanger 402. The cooling medium is ethylene glycol aqueous solution, which stably controls the electrolysis reaction temperature at 0~20℃.
[0041] The intelligent control unit collects temperature, pressure, flow rate, liquid level, current, and voltage parameters in real time through the data acquisition module 503 and transmits them to the DCS control cabinet 501. It sets alarm thresholds for over-temperature (>20℃), over-pressure (>0.2MPa), and abnormal liquid level. When the signal is triggered, the alarm device 502 sounds and lights an alarm, and at the same time automatically cuts off the power supply, stops the liquid supply, and starts the emergency response procedure.
[0042] Operation process: The mixed electrolyte is added to the electrolyte storage tank 201 through the feed port 208. After the liquid level sensor 207 detects that the liquid level has reached the standard, the circulation pump 202 and the temperature control unit are turned on. After the electrolyte circulation is stable and the temperature reaches the standard, power is supplied to the electrolysis module 101 through the positive electrode conductive busbar 103 and the negative electrode conductive busbar 104, and the current density is controlled at 20~100mA / cm 2An electrochemical fluorination reaction is carried out. The gas-liquid mixture produced by the reaction enters the gas-liquid separator 301 through the liquid outlet 106 for separation. The liquid phase is refluxed, and the gas phase is condensed and collected as perfluorooctane product. The by-product hydrogen is purified and discharged. The system operates continuously with a current efficiency of over 85% and a perfluorooctane purity of 99.8%. When a single module is under maintenance, the corresponding flow regulating valve 204 and power supply switch are closed, while the other three modules operate normally, and the continuity of production is not affected.
[0043] Example 2
[0044] Combined with appendix Figure 1 Based on production capacity requirements, the modular electrolysis unit will be expanded to 8 electrolysis modules 101, and the power cabinet 102 will be lengthened accordingly. The remaining structure and component models will remain unchanged, and the volume of the electrolyte storage tank 201 will be adjusted to 20m³. 3 The flow rate of circulating pump 202 was increased to 50m³. 3 / h, 8 branch liquid supply pipes 206 independently supply liquid and control each, doubling the system capacity, the operating parameters of each module are independently monitored, the operating stability and product purity are consistent with Example 1, and there are no abnormalities such as leakage or alarm.
[0045] The above are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
Claims
1. A modular organic electrochemical fluorination electrolysis system, characterized in that, It includes a modular electrolysis unit, an electrolyte circulation supply unit, a gas-liquid separation and recovery unit, a temperature control unit, and a control unit; The modular electrolysis unit is composed of several independent electrolysis modules (101) connected in series / parallel. Each group of electrolysis modules (101) has the same structure and can be independently disassembled and operated. The electrolyte circulation supply unit, gas-liquid separation and recovery unit, and temperature control unit are respectively connected to the modular electrolysis unit. The control unit is electrically connected to the modular electrolysis unit, the electrolyte circulation supply unit, the gas-liquid separation and recovery unit, and the temperature control unit, respectively.
2. The modular organic electrochemical fluorination electrolysis system according to claim 1, characterized in that, The modular electrolysis unit includes multiple electrolysis modules (101). The electrolysis modules (101) adopt a pressure filter type single-pole parallel structure. The electrolysis modules (101) are respectively provided with an inlet (105) and an outlet (106).
3. The modular organic electrochemical fluorination electrolysis system according to claim 1, characterized in that, Multiple electrolysis modules (101) are connected to each other via a positive conductive bus (103) and a negative conductive bus (104). The positive conductive bus (103) is connected to the anode of the electrolysis module (101), and the negative conductive bus (104) is connected to the cathode of the electrolysis module (101). The other end of the positive conductive bus (103) is connected to the positive terminal of the power cabinet (102), and the other end of the negative conductive bus (104) is connected to the negative terminal of the power cabinet (102).
4. The modular organic electrochemical fluorination electrolysis system according to claim 1, characterized in that, The electrolyte circulation supply unit includes an electrolyte storage tank (201), a feeding port (208) on the electrolyte storage tank (201), and a liquid level sensor (207) on the electrolyte storage tank (201).
5. The modular organic electrochemical fluorination electrolysis system according to claim 4, characterized in that, The electrolyte circulation supply unit also includes a magnetically driven anti-corrosion circulation pump (202), a filter (203), and a branch supply pipe (206) that are sequentially connected to the electrolyte storage tank (201). The branch supply pipe (206) is connected to each group of electrolysis modules (101) respectively. A flow sensor (205) and a flow regulating valve (204) are installed on the pipeline connecting the branch supply pipe (206) and the electrolysis module (101).
6. The modular organic electrochemical fluorination electrolysis system according to claim 5, characterized in that, The gas-liquid separation and recovery unit includes a gas-liquid separator (301), the upper end of which is connected to a gas condenser (302), and the lower end of which is connected to a liquid phase reflux pipe (303), which is connected to an electrolyte storage tank (201).
7. A modular organic electrochemical fluorination electrolysis system according to claim 6, characterized in that, The gas-liquid separator (301) is equipped with a pressure sensor (305) and a liquid level monitoring sensor (304).
8. The modular organic electrochemical fluorination electrolysis system according to claim 7, characterized in that, The temperature control unit includes an inlet heat exchanger (401) and an outlet heat exchanger (402). The inlet heat exchanger (401) is located on the pipeline between the electrolyte storage tank (201) and the magnetically driven anti-corrosion circulating pump (202). One end of the outlet heat exchanger (402) is connected to the feed port of the gas-liquid separator (301), and the other end of the outlet heat exchanger (402) is connected to the electrolysis module (101).
9. A modular organic electrochemical fluorination electrolysis system according to claim 7, characterized in that, The temperature control unit also includes a heat exchange coil and a temperature sensor (403); the heat exchange coil is embedded inside the gas-liquid separator (301) housing and the electrolyte storage tank (201) respectively, and the cooling medium circulator uses ethylene glycol aqueous solution as the cooling medium; the temperature sensor (403) is respectively installed on the pipeline of the electrolysis module (101), the electrolyte storage tank (201) and the gas-liquid separator (301), and the temperature sensor (403) is electrically connected to the control unit (5).
10. A modular organic electrochemical fluorination electrolysis system according to claim 7, characterized in that, The energy control unit includes an alarm device (502), a DCS control cabinet (501), and a data acquisition module (503) connected in sequence. The data acquisition module (503) is electrically connected to the modular electrolysis unit, the electrolyte circulation supply unit, the gas-liquid separation and recovery unit, and the temperature control unit, respectively.