Test equipment and control method thereof

Abstract

The invention relates to test equipment and a control method thereof. The glass-lined reaction kettle comprises a reaction kettle body, a stirring device is arranged in the reaction kettle body, and the reaction kettle body is further provided with a reaction kettle feeding port and a reaction kettle discharging port; the cooler comprises an inlet end, a first outlet end and a second outlet end, a pipeline is arranged between the inlet end of the cooler and the discharge port of the reaction kettle, a pipeline is arranged between the inlet end of the cooler and the discharge port of the reaction kettle, and the first outlet end of the cooler is communicated with the reaction kettle through the pipeline; the cooler is used for condensing the gas-phase material into a liquid-phase material; and the storage tank is connected with the cooler and is used for receiving the liquid-phase material from the second outlet end, and part of the gas-phase material which cannot be liquefied returns to the glass-lined reaction kettle through the first outlet end to be rectified again. The device can meet the test requirements of automatic control, accurate temperature and pressure monitoring, anti-corrosion stirring, efficient rectification capacity and the like.

Description

Technical Field

[0001] The present invention relates to the technical field of test equipment, and in particular to a test equipment and its control method. Background Art

[0002] In the pre - batch production tests in fields such as chemical industry, medicine, and pesticides, it is usually necessary to mix, heat, cool, and perform rectification separation on various materials under a controlled environment. Existing experimental devices often have difficulty in taking into account high - precision temperature and pressure control, relatively flexible automatic feeding and stirring schemes, and efficient rectification processes. At the same time, during stirring with traditional equipment, the bottom materials may adhere to the wall or be burnt, and additional scraping devices or anti - corrosion materials are required to adapt to various corrosive media. Summary of the Invention

[0003] Therefore, the present invention provides a test equipment and its control method, which can meet the test requirements such as automated operation, precise temperature and pressure monitoring, anti - corrosion stirring, and efficient rectification ability.

[0004] To solve the above - mentioned technical problems, the present invention provides a test equipment, including a frame, on which are provided: A glass - lined reactor, including a reactor body, in which a stirring device is arranged, and the reactor body is also provided with a reactor feed inlet and a reactor discharge outlet; A cooler, the cooler includes an inlet end, a first outlet end, and a second outlet end. A pipeline is arranged between the inlet end of the cooler and the reactor discharge outlet. The first outlet end of the cooler is connected to the reactor body through the pipeline. The cooler is used to allow the material in the glass - lined reactor to enter the cooler through the pipeline when it reaches the rectification process point, so that the gaseous material is condensed into a liquid material; A storage tank, connected to the cooler, for receiving the liquid material from the second outlet end. Part of the gaseous material that cannot be liquefied returns to the glass - lined reactor through the first outlet end for re - rectification; An integrated control cabinet, used to control the start and stop of the glass - lined reactor, monitor the pressure and temperature inside it, and control the actions of the cooler and the stirring device.

[0005] In one embodiment of the present invention, a pneumatic bottom valve is arranged at the bottom end of the reactor body, which is used to empty the remaining material in the reactor body after the reaction ends.

[0006] In one embodiment of the present invention, the reactor body is wrapped with an outer jacket, and a temperature - measuring device is arranged at the bottom of the reactor body.

[0007] In an embodiment of the present invention, an explosion-proof disc and a pressure gauge are provided at the top of the reactor body, and the explosion-proof disc is connected to a lined tetrafluoro safety valve.

[0008] In an embodiment of the present invention, a gas channel valve is provided on the pipeline.

[0009] In an embodiment of the present invention, the stirring device includes a stirring drive device provided at the top of the reactor body and a stirring shaft connected to the drive end of the stirring drive device and extending into the reactor body. Paddle-type stirring blades and scrapers are installed on the stirring shaft, and the surface of the scraper is covered with an anti-corrosion material to prevent the material from sticking to the wall or bottom of the reactor body or burning.

[0010] In an embodiment of the present invention, a three-way pipe is further included. One end of the three-way pipe is connected to the cooling outlet of the cooler, and the other two ends of the three-way pipe are respectively configured as the first outlet end and the second outlet end.

[0011] In an embodiment of the present invention, the cooler adopts a diaphragm heat exchanger.

[0012] The present invention also provides a control method for a test device. Based on the test device described above, the control method includes: Input the preset process parameters including pressure and temperature into the integrated control cabinet, and start the glass-lined reactor and the stirring device. The material enters the reactor body through the reactor feed port. While carrying out the stirring reaction in the reactor body, the pressure and temperature are monitored in real time through the integrated control cabinet. The integrated control cabinet automatically adjusts the operating conditions of the cooler and the rotation speed of the stirring device according to the monitored values of temperature, pressure and flow rate. When the reaction conditions meet the rectification requirements, control to open the gas channel valve provided on the pipeline, so that the gas-phase material enters the cooler through the inlet end of the cooler for condensation, and part of the gas-phase material that cannot be liquefied returns to the glass-lined reactor through the first outlet end for re-rectification. The liquid-phase material output from the second outlet end of the cooler enters the storage tank for collection. After the reaction is completed, close the pipeline valve and stop the stirring device, and open the pneumatic bottom valve to drain the remaining material in the reactor body.

[0013] The above technical solutions of the present invention have the following advantages compared with the prior art: An experimental device and its control method according to the present invention achieve a modular layout of an enamel reaction kettle, a cooler, a storage tank, and an integrated control cabinet in terms of structure. Combined with a mobile rack, it can be flexibly applied in different experimental scenarios and is also convenient for future maintenance and upgrading. By the integrated control cabinet, the temperature, pressure, and flow rate are monitored in real time and precisely controlled, enabling the reaction and rectification processes to proceed efficiently within a safe range and effectively reducing the incidence of accidents.

[0014] The present invention adopts a collaborative design of a stirring device and a pneumatic bottom valve, which can not only prevent the material from sticking to the wall or burning at the bottom of the reaction kettle, but also quickly empty the remaining material after the reaction ends, improving the efficiency of subsequent operations and cleaning. The cooperation of the cooler, pipeline valves, and three-way pipes realizes the full separation and cyclic rectification of gas-liquid two phases, greatly improving the experimental efficiency and material utilization rate, and meeting the multiple requirements of small-batch pre-experiments in fields such as chemical industry, medicine, and pesticides. Brief Description of the Drawings

[0015] In order to make the content of the present invention easier to be clearly understood, the present invention will be further described in detail below according to specific embodiments of the present invention in conjunction with the drawings.

[0016] Figure 1 It is a front view schematic diagram of the overall structure of an experimental device of the present invention.

[0017] Figure 2 It is a top view structural schematic diagram of the whole of an experimental device of the present invention.

[0018] Figure 3 It is a schematic installation diagram of an explosion-proof film of the present invention.

[0019] Figure 4 It is a schematic diagram of the cooler structure of the present invention.

[0020] Explanation of the reference numerals in the drawings of the specification: 1. Enamel reaction kettle; 11. Reaction kettle body; 12. Reaction kettle feed inlet; 13. Reaction kettle discharge outlet; 14. Pneumatic bottom valve; 15. Outer jacket; 16. Temperature measuring device; 17. Explosion-proof film; 18. Pressure gauge; 19. Teflon safety valve; 2. Stirring device; 21. Stirring drive device; 22. Stirring shaft; 23. Paddle-type stirring blade; 24. Scraper; 3. Cooler; 31. Inlet end; 32. Three-way pipe; 321. First outlet end; 322. Second outlet end; 4. Storage tank; 5. Pipeline; 51. Gas passage valve; 6. Explosion-proof film; 7. Integrated control cabinet; 8. Rack; 81. Mobile roller. Specific Embodiments

[0021] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments, so that those skilled in the art can better understand the present invention and be able to implement it, but the specific embodiments cited are not intended to limit the present invention.

[0022] In the present invention, when directions (up, down, left, right, front, and back) are described, it is only for the convenience of describing the technical solution of the present invention, rather than indicating or implying that the technical features referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention.

[0023] In the present invention, the meaning of "several" is one or more, the meaning of "multiple" is two or more, and "greater than", "less than", "exceeding", etc. are understood to exclude the present number; "above", "below", "within", etc. are understood to include the present number. In the description of the present invention, if "first" and "second" are described, they are only used for the purpose of distinguishing technical features, and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features or implicitly indicating the sequence relationship of the indicated technical features.

[0024] In the present invention, unless otherwise clearly defined, words such as "set", "installed", "connected", etc. should be understood in a broad sense. For example, they can be directly connected, or indirectly connected through an intermediate medium; they can be fixedly connected, or detachably connected, or integrally formed; they can be mechanically connected, or electrically connected or capable of communicating with each other; they can be the communication inside two components or the interaction relationship between two components. Those skilled in the art can reasonably determine the specific meaning of the above words in the present invention in combination with the specific content of the technical solution.

[0025] Referring to Figure 1 、 Figure 2 As shown, a test device of the present invention includes a frame 8, and moving rollers 81 are provided at the bottom of the frame 8. The following are provided on the frame 8: A glass-lined reactor 1, including a reactor body 11. A stirring device 2 is provided inside the reactor body 11. The reactor body 11 is also provided with a reactor feed port 12 and a reactor discharge port 13; Cooler 3, the cooler 3 includes an inlet end 31, a first outlet end 321 and a second outlet end 322. A pipeline 5 is provided between the inlet end 31 of the cooler 3 and the reaction kettle discharge port 13. The cooler 3 is used to enable the material in the glass-lined reaction kettle 1 to enter the cooler 3 through the pipeline 5 when it reaches the rectification process point, so that the gaseous material is condensed into a liquid material; Storage tank 4, connected to the cooler 3, is used to receive the liquid material from the second outlet end 322. Part of the gaseous material that cannot be liquefied returns to the glass-lined reaction kettle 1 through the first outlet end 321 for rectification again; Integrated control cabinet 7, which is used to control the start and stop of the glass-lined reaction kettle 1 and monitor the pressure and temperature inside it, and control the actions of the cooler 3 and the stirring device 2.

[0026] In one embodiment, a pneumatic bottom valve 14 is provided at the bottom end of the reaction kettle body 11, which is used to empty the remaining material in the reaction kettle body 11 after the reaction. By adding a pneumatic bottom valve 14 at the bottom end of the reaction kettle body 11, the automatic emptying of the remaining material in the reaction kettle body 11 after the reaction is realized. Due to the use of pneumatic control, the kettle body can be quickly emptied in a short time, effectively improving safety, reducing the pollution risk caused by residues, and shortening the preparation time for re-feeding or cleaning, meeting the dual requirements of operation efficiency and safety protection.

[0027] In one embodiment, the reaction kettle body 11 is wrapped with an outer jacket 15, and a temperature measuring device 16 (such as a thermometer) is provided at the bottom of the reaction kettle body 11. By providing an outer jacket 15 outside the reaction kettle body 11 for introducing heating or cooling media, the reaction temperature can be more accurately regulated. At the same time, by adding a temperature measuring device 16 at the bottom of the kettle, the temperature distribution of the material in the kettle can be monitored in real time and accurately, facilitating the integrated control cabinet 7 to perform heating or cooling operations in a timely manner. More uniform heat transfer can be achieved, the reaction conditions can be stabilized, and temperature overshoot or local overheating can be avoided, helping to improve the reproducibility and safety of the experiment.

[0028] In one embodiment, refer to Figure 3As shown, an explosion-proof film 6 (0.25MPa) and a pressure gauge 18 are provided at the top of the reactor body 11. The explosion-proof film 6 is connected to a lined tetrafluoro safety valve 19. An explosion-proof film 6 and a pressure gauge 18 are added to the top of the reactor body 11, and pressure release and protection are carried out through the lined tetrafluoro safety valve 19. This structure helps to relieve pressure in a timely manner when abnormal pressure rise or overpressure occurs in the kettle, protecting the safety of the equipment and operators; the use of the lined tetrafluoro safety valve 19 can prevent corrosive materials from damaging the valve body, extend the service life of the device and reduce potential safety hazards.

[0029] In one embodiment, a gas channel valve 51 is provided on the pipeline 5. The gas phase channel can be opened or closed as needed to achieve flexible switching and automatic adjustment. When the material reaches the rectification process point, the operator or the control system can timely adjust the channel valve to ensure that the material smoothly enters the cooler 3 for gas-liquid separation, improving the rectification efficiency and reducing unnecessary energy consumption.

[0030] In one embodiment, the stirring device 2 includes a stirring drive device 21 provided at the top of the reactor body 11 and a stirring shaft 22 connected to the drive end of the stirring drive device 21 and extending into the reactor body 11. A paddle-type stirring blade 23 and a scraper 24 are installed on the stirring shaft 22. The surface of the scraper 24 is covered with an anti-corrosion material (such as tetrafluoro) to prevent the material from sticking to the wall or bottom of the reactor body 11 or burning.

[0031] The stirring device 2 uses the paddle-type stirring blade 23 and the scraper 24 in combination. With the scraper 24 whose surface is covered with an anti-corrosion material, it can effectively reduce the phenomenon of the material sticking to the wall or bottom of the kettle during the reaction process. The paddle-type stirring blade 23 can generate strong flow to fully mix the material; the scraper 24 runs close to the kettle wall and removes the possible adhered solids or lumps through mechanical scraping, further improving the stirring uniformity and increasing the adaptability of the device to various corrosive materials.

[0032] In one embodiment, a three-way pipe 32 is further included. One end of the three-way pipe 32 is connected to the cooling outlet of the cooler 3, and the other two ends of the three-way pipe 32 are respectively configured as the first outlet end 321 and the second outlet end 322. It can simplify the device layout, shorten the pipeline 5 route, and effectively reduce the transmission loss during the gas-liquid separation process; at the same time, the unliquefied gas phase discharged from the first outlet end 321 can be returned to the reactor for re-rectification to improve the separation efficiency, and the second outlet end 322 can transport the liquid phase material formed by condensation to the storage tank 4 for convenient subsequent collection and processing.

[0033] In one embodiment, refer to Figure 4As shown, the cooler 3 adopts a plate heat exchanger. By improving the heat transfer efficiency and heat exchange area, the gas-liquid phase change is accelerated. Optionally, the structure of the plate heat exchanger disclosed in the publication number CN 117419597 A is selected.

[0034] This embodiment also provides a control method for the test equipment. Based on the test equipment described above, the control method includes: S1. Input the preset process parameters including pressure and temperature into the integrated control cabinet 7, and start the glass-lined reactor 1 and the stirring device 2. The material enters the reactor body 11 through the reactor feed port 12.

[0035] The integrated control cabinet 7 is controlled by PLC, and can control the opening or closing of the feed valve according to the set feeding rate, and perform dynamic correction according to the pressure and temperature detected in real time. Diluent or catalyst can be introduced timely during the feeding process.

[0036] S2. While carrying out the stirring reaction in the reactor body 11, the pressure and temperature are monitored in real time through the integrated control cabinet 7. The integrated control cabinet 7 automatically adjusts the operating conditions of the cooler 3 and the rotation speed of the stirring device 2 according to the monitored values of temperature, pressure and flow rate.

[0037] It should be noted that after the material enters the reactor, the stirring device 2 starts to work at the preset rotation speed to achieve full mixing of the material. Since the integrated control cabinet 7 will feedback the data of the pressure gauge and thermometer to the internal control system in real time, during the stirring reaction process, if the detected temperature or pressure deviates from the established range, the control system will quickly adjust the supply amount of the outer jacket 15 or the corresponding heat source and cold source, so that the reactor always remains in the optimal reaction range. At the same time, according to the flow rate monitoring value, the stirring state and the gas-liquid phase distribution are judged, and the operating conditions of the cooler 3 and the rotation speed of the stirring device 2 are automatically adjusted to avoid local overheating or blockage.

[0038] S3. When the reaction conditions meet the rectification requirements, control to open the gas channel valve 51 provided on the pipeline 5, so that the gas-phase material enters the cooler 3 through the inlet end 31 of the cooler 3 for condensation, and part of the gas-phase material that cannot be liquefied returns to the glass-lined reactor 1 through the first outlet end 321 for rectification again.

[0039] It should be noted that when the monitoring data shows that the reaction conditions have met the requirements of rectification, an instruction is sent through the integrated control cabinet 7 to open the gas passage valve 51 provided on the pipeline 5, so that the gas-phase material enters the inlet end 31 of the cooler 3 for condensation. If some gases cannot be effectively liquefied in the cooler 3, they can return to the reaction kettle body 11 from the first outlet end 321 for re-rectification, thereby improving the separation efficiency within a cycle loop. At this time, the integrated control cabinet 7 combines the temperature, pressure, and flow monitoring information to automatically adjust the cooling intensity of the cooler 3, such as controlling the flow rate and temperature range of cooling water or refrigerant, and comprehensively balancing the cooling load and the requirements for vacuum degree or pressure to achieve the best gas-liquid separation effect.

[0040] S4. The liquid-phase material output from the second outlet end 322 of the cooler 3 enters the storage tank 4 for collection; S5. After the reaction is completed, close the valve of the pipeline 5 and stop the stirring device 2, and open the pneumatic bottom valve 14 to drain the remaining material in the reaction kettle body 11.

[0041] When the reaction and rectification processes are all completed, the pipeline 5 valve is closed and the stirring device 2 is stopped through the integrated control cabinet 7, and the pneumatic bottom valve 14 provided at the bottom of the reaction kettle is opened to discharge the remaining material in the kettle. The pneumatic operation mode makes the entire emptying process more efficient and reduces the risk of manual discharging in high-temperature, high-pressure, or corrosive environments. At the same time, this step can be connected to the subsequent cleaning process, facilitating the timely replacement of materials or conducting multi-batch tests.

[0042] Exemplarily, one of two different types of catalysts can be selected for the stirring reaction carried out in the reaction kettle body 11, namely palladium-carbon catalyst or Raney nickel catalyst. Palladium-carbon catalyst and Raney nickel catalyst are mainly used in various hydrogenation (or dehydrogenation) reactions, and the corresponding materials usually require reaction substrates or raw materials to be catalytically converted under specific conditions. In addition, the choice of the catalyst can be determined according to specific process requirements, such as the type of target product, reaction rate, and tolerance to impurities.

[0043] When using the palladium-carbon catalyst, the preset process parameters include a reaction pressure range of 0.2 - 1.0 MPa and a reaction temperature range of 50 - 150 °C. After inputting and setting the preset pressure and temperature values through the integrated control cabinet 7, precise temperature control is achieved through the outer jacket 15, and the pressure gauge 18 and explosion-proof sheet 6 are used to monitor and ensure that the pressure in the kettle is within the set value. Under these conditions, the palladium-carbon catalyst can effectively promote the progress of specific chemical reactions, shorten the reaction cycle, and improve the selectivity of the target product.

[0044] When using a Raney nickel catalyst, the preset process parameters include a reaction pressure range of 0.3 - 1.2 MPa and a reaction temperature range of 80 - 180 °C. The integrated control cabinet 7 will also automatically adjust the flow rate of the heating or cooling medium in the outer jacket 15 according to the monitored values of temperature, pressure, and flow rate at this time, and control the rotation speed of the stirring device 2 to ensure that the Raney nickel catalyst continuously exhibits stable catalytic activity at a relatively high temperature and appropriate pressure. When the rectification requirements are met, the gas channel valve 51 is opened, and the gas-phase stream can be condensed via the cooler 3. The uncondensed part returns to the glass-lined reactor 1 for re-rectification, thereby achieving more efficient separation and collection of the target product.

[0045] The above two catalysts are only used as the exemplary application scope of the present invention in different scenarios. In actual applications, other types of metal catalysts or acidic catalysts can also be replaced according to the process objectives, and the preset values of the reaction pressure and temperature can be adjusted accordingly. The test equipment described in the present invention, in combination with different catalysts and diverse process parameters, can achieve precise, flexible, and efficient test operations in the early small-batch experiments in the fields of medicine, chemical industry, pesticides, and fine chemicals.

[0046] Finally, it should be noted that the above specific embodiments are only used to illustrate the technical solutions of the present invention and are not restrictive. Although the present invention has been described in detail with reference to the examples, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention, and they should all be covered within the scope of the claims of the present invention.

Claims

1. An experimental device, characterized in that, It includes a frame (8), and the following are arranged on the frame (8): A glass-lined reactor (1), which includes a reactor body (11). A stirring device (2) is arranged inside the reactor body (11). The reactor body (11) is also provided with a reactor feed inlet (12) and a reactor discharge outlet (13); A cooler (3), which includes an inlet end (31), a first outlet end (321) and a second outlet end (322). A pipeline (5) is arranged between the inlet end (31) of the cooler (3) and the reactor discharge outlet (13). A pipeline (5) is arranged between the inlet end (31) of the cooler (3) and the reactor discharge outlet (13). The first outlet end (321) of the cooler (3) is communicated with the reactor body (11) through the pipeline (5). The cooler (3) is used to enable the gas-phase material to condense into a liquid-phase material by entering the cooler (3) through the pipeline (5) when the material in the glass-lined reactor (1) reaches the rectification process point; A storage tank (4), which is connected to the cooler (3) and is used to receive the liquid-phase material from the second outlet end (322). Part of the non-liquefiable gas-phase material returns to the glass-lined reactor (1) through the first outlet end (321) for re-rectification; An integrated control cabinet (7), which is used to control the start and stop of the glass-lined reactor (1), monitor the pressure and temperature inside it, and control the actions of the cooler (3) and the stirring device (2).

2. An experimental device according to claim 1, characterized in that, A pneumatic bottom valve (14) is arranged at the bottom end of the reactor body (11) and is used to empty the remaining material in the reactor body (11) after the reaction ends.

3. An experimental device according to claim 1, characterized in that, The outside of the reactor body (11) is wrapped with an outer jacket (15), and a temperature measuring device (16) is arranged at the bottom of the reactor body (11).

4. An experimental device according to claim 1, characterized in that, An explosion-proof disc (6) and a pressure gauge (18) are arranged at the top end of the reactor body (11), and the explosion-proof disc (6) is connected to a lined tetrafluoro safety valve (19).

5. An experimental device according to claim 1, characterized in that, A gas passage valve (51) is arranged on the pipeline (5).

6. An experimental device according to claim 1, characterized in that, The stirring device (2) includes a stirring drive device (21) arranged at the top of the reactor body (11) and a stirring shaft (22) connected to the drive end of the stirring drive device (21) and extending into the reactor body (11). A paddle-type stirring blade (23) and a scraper (24) are installed on the stirring shaft (22). The surface of the scraper (24) is covered with an anti-corrosion material and is used to prevent the material from sticking to the wall or bottom of the reactor body (11) or burning and charring.

7. An experimental device according to claim 1, characterized in that, It also includes a three-way pipe (32). One end of the three-way pipe (32) is connected to the cooling outlet of the cooler (3), and the other two ends of the three-way pipe (32) are respectively configured as the first outlet end (321) and the second outlet end (322).

8. An experimental device according to claim 1, characterized in that, The cooler (3) adopts a diaphragm heat exchanger.

9. A control method for a test device, characterized in that, Based on the test equipment according to any one of claims 1-8, the control method includes: Input the preset process parameters including pressure and temperature into the integrated control cabinet (7), and start the glass-lined reactor (1) and the stirring device (2). The material enters the reactor body (11) through the reactor feed inlet (12). While carrying out the stirring reaction in the reactor body (11), the pressure and temperature are monitored in real time through the integrated control cabinet (7). The integrated control cabinet (7) automatically adjusts the operating conditions of the cooler (3) and the rotation speed of the stirring device (2) according to the monitored values of temperature, pressure and flow rate. When the reaction conditions meet the rectification requirements, control to open the gas passage valve (51) provided on the pipeline (5), so that the gas-phase material enters the cooler (3) through the inlet end (31) of the cooler (3) for condensation. Part of the gas-phase material that cannot be liquefied returns to the glass-lined reactor (1) through the first outlet end (321) for re-rectification. The liquid-phase material output from the second outlet end (322) of the cooler (3) enters the storage tank (4) for collection. After the reaction is completed, close the valve of the pipeline (5) and stop the stirring device (2), and open the pneumatic bottom valve (14) to empty the remaining material in the reactor body (11).

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