Continuous adiabatic test system, method and equipment for thermal stability of substances

Abstract

Embodiments of the present disclosure provide a continuous adiabatic test system, method, and device for the thermal stability of substances. The system includes: a feeding device for providing test materials to the test cell; a cell heater for heating the test cell so that the test materials start a chemical reaction; a material recovery tank for recovering the reactants generated during the chemical reaction of the test materials; and an analysis device for analyzing the reactants to determine the conversion rate of the test materials. In this way, a test cell can be customized for experiments according to actual conditions, and a test method with real-time analysis can be carried out, which saves time and effort, is powerful in function, has a small thermal inertia, and can use continuous process simulation experiments to measure the thermal stability of substances or measure relevant data and develop technologies for runaway reactions.

Description

Technical Field

[0001] The present disclosure relates to the field of adiabatic testing, and particularly to the field of thermal stability testing technology. Background Art

[0002] At present, the adiabatic testing method is generally used in China and even the world to measure the thermal stability data of substances. However, the simulation tests are all based on intermittent or semi-intermittent working conditions, that is, it is impossible to feed materials or recycle materials during the test. Therefore, there is no reliable data support for continuous working conditions. In later process design, hazard analysis, production and other processes, overprotection may occur based on the thermal safety data measured in semi-intermittent or intermittent conditions, resulting in a large amount of manpower and material resources. Therefore, how to directly obtain the thermal stability test data of substances in a continuous process is of crucial significance, and there is no reliable adiabatic testing method for the thermal stability of substances based on a continuous process in the prior art. Summary of the Invention

[0003] The present disclosure provides a continuous adiabatic testing system, method and equipment for the thermal stability of substances.

[0004] According to a first aspect of the present disclosure, a continuous adiabatic testing system for the thermal stability of substances is provided. The system includes: a feeding device, a high-pressure reaction kettle, a material recovery tank, and an analysis device. A test pool is placed inside the high-pressure reaction kettle, and a pool heater is wrapped outside the test pool. The feeding device, the material recovery tank, and the analysis device are all connected to the test pool, wherein:

[0005] The feeding device is used to provide test materials for the test pool;

[0006] The pool heater is used to heat the test pool so that the test materials start a chemical reaction;

[0007] The material recovery tank is used to recover the reactants generated during the chemical reaction of the test materials;

[0008] The analysis device is used to analyze the reactants to determine the conversion rate of the test materials.

[0009] In the above aspect and any possible implementation manner, a further implementation manner is provided. The system further includes: a gas pipeline and a liquid pipeline,

[0010] The gas pipeline is connected between the top of the test pool and the top of the material recovery tank,

[0011] The liquid pipeline is connected between the bottom of the test pool and the middle and lower part of the material recovery tank.

[0012] For the aspects and any possible implementation manners as described above, a further implementation manner is provided. A first heat insulation layer, an external tracking heater, and a second heat insulation layer are further provided inside the high-pressure reactor.

[0013] The first heat insulation layer wraps around the periphery of the test cell, and the cell heater is arranged inside the heat insulation layer.

[0014] The external tracking heater wraps around the outside of the first heat insulation layer and is used to heat the first heat insulation layer when the temperature of the first heat insulation layer is lower than the temperature inside the test cell. Among them, both the external tracking heater and the cell heater have openings facing upwards.

[0015] The second heat insulation layer is located inside the high-pressure reactor and outside the external tracking heater.

[0016] For the aspects and any possible implementation manners as described above, a further implementation manner is provided. An internal thermocouple and an external thermocouple are further provided inside the high-pressure reactor.

[0017] The internal thermocouple is inserted inside the test cell and is used to measure the temperature inside the test cell and upload it for recording.

[0018] The external thermocouple is inserted inside the first heat insulation layer and is used to measure the temperature of the first heat insulation layer and upload it for recording.

[0019] For the aspects and any possible implementation manners as described above, a further implementation manner is provided. The system further includes:

[0020] A pipeline thermocouple, a pipeline pressure gauge, a gas-phase space thermocouple, and a liquid-phase space thermocouple;

[0021] The pipeline thermocouple and the pipeline pressure gauge are connected to the gas pipeline and are located at the top of the material recovery tank.

[0022] The pipeline thermocouple is used to measure the temperature on the gas pipeline and upload it for recording;

[0023] The pipeline pressure gauge is used to measure the pressure inside the test cell and upload it for recording;

[0024] The gas-phase space thermocouple and the liquid-phase space thermocouple are both installed inside the material recovery tank and are respectively used to measure the temperature of the gas-phase space and the temperature of the liquid-phase space inside the material recovery tank and upload them for recording.

[0025] For the aspects and any possible implementation manners as described above, a further implementation manner is provided. The system further includes:

[0026] A temperature-tracking heater, wrapped around the periphery of the gas-phase pipeline, the material recovery tank, and the liquid-phase pipeline, is used to start heating when the temperature in the gas-phase pipeline or the material recovery tank is lower than the temperature in the test cell;

[0027] A three-way sampling valve and a stop valve,

[0028] The three-way sampling valve is installed on the liquid-phase pipeline and is connected to the analysis device;

[0029] The stop valve is located at the end of the liquid-phase pipeline, close to the material recovery tank.

[0030] For the aspects and any possible implementation manners as described above, a further implementation manner is provided. The system further includes:

[0031] A kettle cover, a pressure connection pipeline, a pressure sensor, and a pressure control device;

[0032] The kettle cover is sealed with a gasket and fastened with bolts between the kettle cover and the high-pressure reactor;

[0033] One end of the pressure connection pipeline is connected to the kettle cover and extends into the high-pressure reactor, and the other end is connected to the pressure control device;

[0034] The pressure sensor is installed on the pressure connection pipeline. The pressure sensor is used to collect the pressure outside the test cell and upload it for recording;

[0035] The pressure control device, located above the kettle cover, is used to inflate or exhaust gas into the high-pressure reactor through the pressure connection pipeline according to the pressure difference between the pressure outside the test cell and the pressure inside the test cell; and

[0036] The system further includes:

[0037] A magnetic stirrer, the magnetic stirrer is located at the bottom of the high-pressure reactor;

[0038] The magnetic stirrer cooperates with the magnetic stir bar in the test cell to stir the test material in the test cell.

[0039] For the aspects and any possible implementation manners as described above, a further implementation manner is provided. The feeding device includes:

[0040] A feed tank, a feed tank bottom valve, a feed pump, a raw material flow meter, a heat exchanger, and a feed pipeline;

[0041] The feed tank bottom valve is located at the bottom of the feed tank;

[0042] The feed pump is connected to the feed tank bottom valve and the raw material flow meter;

[0043] The heat exchanger is connected to the raw material flowmeter and the feed pipeline;

[0044] The feed pipeline is connected to the top of the test cell.

[0045] According to a second aspect of the present disclosure, there is provided a method for adiabatic testing of the thermal stability of a substance in a continuous process. The method is applicable to a continuous adiabatic testing system for the thermal stability of a substance, the system comprising a feeding device, a high-pressure reactor, a material recovery tank, and an analysis device. A test cell is placed inside the high-pressure reactor and a cell heater is wrapped around the test cell. The feeding device, the material recovery tank, and the analysis device are all connected to the test cell. The method comprises:

[0046] The feeding device provides test materials for the test cell;

[0047] The cell heater heats the test cell so that the test materials start a chemical reaction;

[0048] The material recovery tank recovers the reactants generated during the chemical reaction of the test materials;

[0049] The analysis device analyzes the reactants to determine the conversion rate of the test materials.

[0050] According to a third aspect of the present disclosure, there is provided an electronic device. The electronic device comprises: a memory and a processor, a computer program is stored on the memory, and when the processor executes the program, the method as described above is implemented.

[0051] According to a fourth aspect of the present disclosure, there is provided a computer-readable storage medium, on which a computer program is stored, and when the program is executed by a processor, the method as according to the first aspect and / or the second aspect of the present disclosure is implemented.

[0052] In the present disclosure, a test method that can customize the test cell according to actual situations for experiments and can perform real-time analysis is time-saving and labor-saving, has powerful functions, has a small thermal inertia, and can use a continuous process simulation experiment to measure the thermal stability of a substance or measure relevant data and develop technologies for runaway reactions. Therefore, the thermal stability test data is relatively reliable, and problems such as overprotection, and the consumption of a large amount of manpower and material resources in the later process design, hazard analysis, production, etc. due to the thermal safety data measured based on semi-batch or batch can be avoided.

[0053] It should be understood that the content described in the summary of the invention section is not intended to limit the key or important features of the embodiments of the present disclosure, nor is it used to limit the scope of the present disclosure. Other features of the present disclosure will become easily understood through the following description. BRIEF DESCRIPTION OF THE DRAWINGS

[0054] In conjunction with the accompanying drawings and with reference to the following detailed description, the above and other features, advantages, and aspects of the various embodiments of the present disclosure will become more apparent. The accompanying drawings are used to better understand the solution and do not limit the present disclosure. In the drawings, the same or similar reference numerals denote the same or similar elements, where:

[0055] Figure 1 shows a block diagram of a continuous adiabatic test system for the thermal stability of substances according to an embodiment of the present disclosure;

[0056] Figure 2 shows a block diagram of another continuous adiabatic test system for the thermal stability of substances according to an embodiment of the present disclosure;

[0057] Figure 3 shows a graph of the relationship between temperature and concentration over time in a 15% hydrogen peroxide test material in a continuous adiabatic test method for the thermal stability of substances according to an embodiment of the present disclosure;

[0058] Figure 4 shows a graph of the relationship between the temperature and pressure in the test cell over time in a 15% hydrogen peroxide test material in a continuous adiabatic test method for the thermal stability of substances according to an embodiment of the present disclosure;

[0059] Figure 5 shows a flowchart of a continuous adiabatic test method for the thermal stability of substances according to an embodiment of the present disclosure;

[0060] Figure 6 shows a block diagram of an exemplary electronic device capable of implementing the embodiments of the present disclosure.

[0061] The following Figure 1 and Figure 2 explain the correspondence between the components and the numbers therein:

[0062] 1. Feed tank, 2. Feed tank bottom valve, 3. Feed pump, 4. Raw material flowmeter, 5. Heat exchanger, 6. Feed pipeline, 7. Magnetic stirrer, 8. High-pressure reactor, 9. Reactor cover, 10. Pressure control device, 11. Pressure sensor, 12. Pressure connection pipeline, 13. Test cell, 14. Internal thermocouple, 15. External thermocouple, 16. Cell heater, 17. External tracking heater, 18. First insulation layer, 19. Second insulation layer, 20. Gas phase pipeline, 21. Pipeline thermocouple, 22. Pipeline pressure gauge, 23. Material recovery tank, 24. Gas phase space thermocouple, 25. Liquid phase space thermocouple, 26. Drain valve, 27. Temperature tracking heater, 28. Stop valve, 29. Three-way sampling valve, 30. Liquid phase pipeline, 31. Analysis device, 32. Feeding device. Detailed implementation manners

[0063] To make the objectives, technical solutions and advantages of the embodiments of the present disclosure clearer, the technical solutions in the embodiments of the present disclosure will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present disclosure. Obviously, the described embodiments are some but not all of the embodiments of the present disclosure. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present disclosure without creative efforts shall fall within the scope of protection of the present disclosure.

[0064] In addition, the term "and / or" in this document is merely a description of the association relationship of associated objects, indicating that three relationships may exist. For example, A and / or B may represent: A exists alone, A and B exist simultaneously, and B exists alone. In addition, the character " / " in this document generally represents an "or" relationship between the associated objects before and after.

[0065] Figure 1 The block diagram of the adiabatic test system 100 for the thermal stability of continuous substances according to an embodiment of the present disclosure is shown. The system includes:

[0066] A feeding device 32, a high-pressure reactor 8, a material recovery tank 23, and an analysis device 31. A test cell 13 is placed in the high-pressure reactor 8, and a cell heater 16 is wrapped outside the test cell 13. The feeding device 32, the material recovery tank 23, and the analysis device 31 are all connected to the test cell 13, where:

[0067] The feeding device 32 is used to provide test materials for the test cell 13; various parameters of the test cell 13, such as size, thickness, and pressure resistance, can be freely determined according to actual situations, and the test materials can also vary freely according to test requirements.

[0068] The cell heater 16 is used to heat the test cell 13 so that the test materials start a chemical reaction;

[0069] The material recovery tank 23 is used to recover the reactants generated during the chemical reaction of the test materials; the reactants are the products of the test materials.

[0070] The analysis device 31 is used to analyze the reactants to determine the conversion rate of the test materials. For example, the mass of the test materials participating in the reaction can be determined according to the mass of the reactants, and then based on the initial mass of the test materials, the conversion rate of the test materials can be determined.

[0071] By setting up a feeding device 32, a material recovery tank 23, and an analysis device 31, which are connected to the high-pressure reactor 8, when testing the chemical reaction of the test material in the test tank 13 in the high-pressure reactor 8, it is still possible to supply the test material by using the feeding device 32 while recovering the reactants by using the material recovery tank 23 and analyzing the reactants during the reaction in real time, so as to determine the conversion rate of the test material. And this test method of customizing the test tank 13 according to the actual situation for experiments and being able to conduct real-time analysis saves time and effort, is powerful, has a small thermal inertia, and can use continuous process simulation experiments to measure the thermal stability of substances or measure relevant data and conduct technology development for runaway reactions. Therefore, the thermal stability test data is relatively reliable, and it can avoid problems such as overprotection, and the consumption of a large amount of manpower and material resources in the later process design, hazard analysis, production, etc. due to the thermal safety data measured based on semi-batch or batch processes. For example, the reliable conversion rate obtained through this embodiment is beneficial to accurately obtain the kinetic formula of the runaway reaction.

[0072] As Figure 2 shown, in one embodiment, the system further includes: a gas pipeline 20 and a liquid pipeline 30,

[0073] The gas pipeline 20 is connected between the top of the test tank 13 and the top of the material recovery tank 23,

[0074] The liquid pipeline 30 is connected between the bottom of the test tank 13 and the middle and lower part of the material recovery tank 23.

[0075] By connecting the gas pipeline 20 and the liquid pipeline 30 between the test tank 13 and the material recovery tank 23, the gas-phase and liquid-phase reactants in the test tank 13 can enter the material recovery tank 23 through different pipelines respectively.

[0076] The gas pipeline 20 is located above the liquid pipeline 30. The gas pipeline 20 is connected to the top of the test tank 13, and the liquid pipeline 30 is located at the bottom of the test tank 13.

[0077] As Figure 2 shown, in one embodiment, a first heat-insulating layer 18, an external tracking heater 17, and a second heat-insulating layer 19 are further provided in the high-pressure reactor 8,

[0078] The first heat-insulating layer 18 is wrapped around the periphery of the test tank 13, and the tank heater 16 is arranged in the heat-insulating layer;

[0079] The external tracking heater 17 is wrapped outside the first heat-insulating layer and is used to heat the first heat-insulating layer 18 when the temperature of the first heat-insulating layer 18 is lower than the temperature in the test tank 13; wherein, both the external tracking heater 17 and the tank heater 16 open upward;

[0080] The second heat-insulating layer 19 is located inside the high-pressure reactor 8 and outside the external tracking heater 17.

[0081] The first heat-insulating layer 18, the external tracking heater 17, and the second heat-insulating layer 19 provided inside the high-pressure reactor 8 are all located outside the test cell 13 and are used for heat preservation and heat insulation to ensure that the temperature of the test cell 13 is basically the same as that of other positions inside the high-pressure reactor 8, so as to maintain the adiabatic test environment of the test cell 13.

[0082] The external tracking heater 17 adopts a variable power design. According to the temperature change inside the test cell 13, the heating power of the external tracking heater 17 is quickly adjusted, so as to appropriately heat or stop heating the first heat-insulating layer 18, making the temperature inside and outside the test cell 13 basically the same.

[0083] As Figure 2 shown, in one embodiment, an internal thermocouple 14 and an external thermocouple 15 are further provided inside the high-pressure reactor 8.

[0084] The internal thermocouple 14 is inserted inside the test cell 13 and is used to measure the temperature inside the test cell 13 and upload it for recording.

[0085] The external thermocouple 15 is inserted inside the first heat-insulating layer 18 and is used to measure the temperature of the first heat-insulating layer 18 and upload it for recording.

[0086] By providing the internal thermocouple 14 and the external thermocouple 15 inside the high-pressure reactor 8, the temperature inside the test cell 13 and the temperature of the first heat-insulating layer 18 can be accurately measured respectively. Then, according to the difference between the recorded temperature of the first heat-insulating layer 18 and the temperature inside the test cell 13, the temperature of the first heat-insulating layer 18 is adjusted, so that the temperature of the first heat-insulating layer 18 tracks the change of the temperature inside the test cell 13, and finally the temperature inside and outside the test cell 13 is basically the same.

[0087] Through this embodiment, real-time and rapid acquisition and storage of the temperature at different time points during the thermal stability test can be realized. The change of the temperature inside the test cell is used as one of the data for the continuous thermal stability test of substances, providing useful data for the design of the chemical continuous process. Of course, the temperature change curve inside the test cell is as Figure 4 shown.

[0088] As Figure 2 shown, in one embodiment, the system further includes:

[0089] a pipeline thermocouple 21, a pipeline pressure gauge 22, a gas-phase space thermocouple 24, and a liquid-phase space thermocouple 25;

[0090] The pipeline thermocouple 21 and the pipeline pressure gauge 22 are connected to the gas pipeline 20 and are located at the top of the material recovery tank 23;

[0091] The pipeline thermocouple 21 is used to measure the temperature on the gas pipeline 20 and upload it for recording;

[0092] The pipeline pressure gauge 22 is used to measure the pressure in the test tank 13 and upload it for recording;

[0093] The gas-phase space thermocouple 24 and the liquid-phase space thermocouple 25 are both installed inside the material recovery tank 23 and are respectively used to measure the temperature of the gas-phase space and the liquid-phase space in the material recovery tank 23 and upload it for recording.

[0094] By setting thermocouples and pressure gauges in the gas pipeline 20 and the material recovery tank 23, the temperature and pressure in the gas pipeline 20 and the material recovery tank 23 can be tested, so as to monitor the temperature at different positions in real time, so as to adjust the temperature at different positions in real time so that the temperature at different positions can track the change of the temperature in the test tank 13 and achieve temperature consistency; in addition, the pressure in the test tank 13 can also be tracked and recorded in real time, as one of the thermal stability test data, so as to provide reliable data support for the thermal stability of the materials in the chemical continuous system. Of course, the change curve of the pressure in the test tank is as Figure 4 shown.

[0095] Through this embodiment, the pressure at different time points in the test tank during the thermal stability test can be collected and stored in real time and quickly, providing useful data for the design of the chemical continuous process.

[0096] As Figure 2 shown, in one embodiment, the system further includes:

[0097] A temperature tracking heater 27, which is wrapped around the periphery of the gas pipeline 20, the material recovery tank 23, and the liquid pipeline 30, and is used to turn on the heating when the temperature in the gas pipeline 20 or the material recovery tank 23 is lower than the temperature in the test tank 13; actually, the device wrapped around the periphery of the gas pipeline 20, the material recovery tank 23, and the liquid pipeline 30 is a heat tracing device, and the temperature tracking heater 27 is wrapped around the periphery of the heat tracing device and is used to heat the heat tracing device to achieve heating of the pipeline or the material recovery tank 23; in addition, the heat tracing device may not be integrated, but multiple sections of heat tracing tapes, so as to achieve heating of different positions in the pipeline or the material recovery tank 23 by heating different sections of heat tracing tapes.

[0098] A three-way sampling valve 29 and a stop valve 28,

[0099] The three-way sampling valve 29 is installed on the liquid-phase pipeline 30 and is connected to the analysis device 31;

[0100] The stop valve 28 is located at the end of the liquid-phase pipeline 30, close to the material recovery tank 23.

[0101] The outer side of the material recovery tank 23, the gas-phase pipeline 20, and the liquid-phase pipeline 30 are all wrapped with jackets (i.e., the heat tracing device, Figure 2 not shown in the figure). Therefore, by configuring the temperature tracking heater 27, when the temperature at any position in the gas-phase pipeline 20 or the material recovery tank 23 is lower than the temperature in the test cell 13, heating can be started to heat this position, so that the temperature at each position is basically the same as the temperature in the test cell 13.

[0102] The temperature tracking heater adopts a variable power design, and quickly adjusts the heating power of the temperature tracking heater according to the temperature change in the test cell 13, so as to heat the gas-phase pipeline 20 or the material recovery tank 23, making the temperature at different positions basically the same as the temperature in the test cell 13.

[0103] In addition, by setting the three-way sampling valve 29 and the stop valve 28, after the liquid-phase reactant enters the bottom of the material recovery tank 23 through the liquid-phase pipeline 30, a part of the liquid-phase reactant can be introduced into the analysis device 31 through the three-way sampling valve 29, so that the analysis device 31 can analyze the composition of the liquid-phase reactant and perform relevant determinations of the conversion rate.

[0104] Of course, a three-way sampling valve 29 can also be connected to the gas-phase pipeline 20. At this time, the analysis device 31 can also be connected to the three-way sampling valve 29 on the gas-phase pipeline 20 at the same time, so that a part of the gas-phase reactant can be introduced into the analysis device 31 through the three-way sampling valve 29, enabling the analysis device 31 to analyze the composition of the gas-phase reactant and the liquid-phase reactant at the same time, so as to accurately perform relevant determinations of the conversion rate.

[0105] In one embodiment, the system further includes:

[0106] The kettle cover 9, the pressure connection pipeline 12, the pressure sensor 11 (P2), and the pressure control device 10;

[0107] The kettle cover 9 and the high-pressure reactor 8 are sealed with gaskets and fastened with bolts;

[0108] One end of the pressure connection pipeline 12 is connected to the kettle cover 9, extends into the high-pressure reactor 8, and the other end is connected to the pressure control device 10;

[0109] The pressure sensor 11 is installed on the pressure connection pipeline 12. The pressure sensor 11 is used to collect the external pressure of the test cell 13 and upload it for recording;

[0110] The pressure control device 10 is located above the kettle cover 9. It is used to inflate or exhaust gas into the high-pressure reactor 8 through the pressure connection pipeline 12 according to the pressure difference between the recorded external pressure of the test cell 13 (the pressure collected by the pressure sensor 11) and the internal pressure of the test cell 13 (the pressure collected by the pipeline pressure gauge 22). The internal pressure of the test cell 13 is measured by the pipeline thermocouple 21 on the gas pipeline 20.

[0111] And

[0112] The system further includes:

[0113] A magnetic stirrer 7, which is located at the bottom of the high-pressure reactor 8;

[0114] The magnetic stirrer 7 cooperates with the magnetic stir bar in the test cell 13 to stir the test material in the test cell 13.

[0115] By setting the pressure control device 10 including an electromagnetic valve group, the electromagnetic valve group can be controlled to charge or discharge nitrogen according to the pressure difference change inside and outside the test cell 13. As the chemical reaction of the test material in the test cell 13 proceeds and the temperature rises, the pressure in the test cell 13 continuously increases, and nitrogen is introduced into the gas phase space between the test cell 13 and the high-pressure reactor 8 to supplement the pressure (specifically, when the pressure in the test cell 13 is greater than the external pressure of the test cell 13, the high-pressure reactor 8 is filled with gas, and when the pressure in the test cell 13 is lower than the external pressure of the test cell 13, the high-pressure reactor 8 is exhausted. This gas filling or exhausting process only fills or exhausts the space outside the test cell 13 in the high-pressure reactor 8); when cooling after the test is completed, the pressure in the test cell 13 gradually decreases, and the nitrogen in the gas phase space between the test cell 13 and the high-pressure reactor 8 is discharged (nitrogen charging, nitrogen discharging, and measuring the external pressure of the sample cell are all carried out through the pipeline 12). The pressure difference between inside and outside the test cell 13 is maintained between 0.1 - 0.5 MPa, realizing approximate synchronization of the pressures inside and outside the test cell 13.

[0116] The gas phase space between the test cell 13 and the high-pressure reactor 8 is filled with a thermally inert material to reduce the influence of heat convection caused by gas charging and discharging, and further increase the reliability of the adiabatic environment.

[0117] Maintaining a certain threshold for the pressure between inside and outside the test cell 13 is for the side wall of the test cell 13 to be lighter and thinner, so that more heat supplied to the test cell 13 is absorbed by the test material inside the test cell 13 rather than the test cell 13 itself, and thus the thermal inertia is lower.

[0118] In addition, the magnetic stirrer 7 can be used to stir the test material in the test cell 13 by magnetic force.

[0119] In one embodiment, the feeding device 32 includes:

[0120] a feeding tank 1, a bottom valve 2 of the feeding tank, a feeding pump 3, a raw material flowmeter 4, a heat exchanger 5, and a feeding pipeline 6;

[0121] The bottom valve 2 of the feeding tank is located at the bottom of the feeding tank;

[0122] The feeding pump 3 is connected to the bottom valve 2 of the feeding tank and the raw material flowmeter 4;

[0123] The heat exchanger 5 is connected to the raw material flowmeter 4 and the feeding pipeline 6;

[0124] The feeding pipeline 6 is connected to the top of the test cell 13.

[0125] By configuring the feeding tank 1, the bottom valve 2 of the feeding tank, the feeding pump 3, the raw material flowmeter 4, the heat exchanger 5, and the feeding pipeline 6, test materials can be provided for the test cell 13.

[0126] In addition, there can be multiple feeding devices 32. When the feeding device 32, the gas pipeline 20, and the liquid pipeline 30 are connected to the test cell 13, through-wall joints are provided on the openings on the side wall of the high-pressure reactor 8, and the pipelines on both sides of the opening are connected to the through-wall joints and fixed by ferrule nuts (i.e., standard Swagelok ferrules).

[0127] Through this embodiment, it is possible to realize the real-time and rapid acquisition and storage of the feeding flow rates at different time points during the thermal stability test by using the raw material flowmeter 4 and the storage device, providing useful data for the design of the chemical continuous process.

[0128] According to actual needs, the heat exchanger can be a sample heater or cooler provided on the liquid and gas feeding pipelines, or a gas-liquid mixer, etc. can also be set according to specific working conditions. For example: if a liquid-phase reaction needs to be carried out, but the test material provided by the feeding tank is a gas at room temperature, then the heat exchanger is a cooler.

[0129] In addition, it should be noted that the system of the present disclosure also has a control device and a storage device, so as to store various data uploaded by the sensors by using the storage device, and issue control commands generated based on various data uploaded by the sensors, such as heating commands, gas charging commands, gas discharging commands, etc. The control device and the storage device can be freely set by those skilled in the art according to actual needs, and the disclosure does not make any restrictions.

[0130] The following Figures 1 to 4 further describes the embodiments of the present disclosure:

[0131] Test cell 13

[0132] The content volume of test cell 13 is 0.1 - 0.12 L, such as 0.11 L, the wall thickness is 0.3 - 0.5 mm, such as 0.33 mm, the maximum differential pressure it can withstand is 0.5 MPa, the design temperature is 300 - 400 °C, such as 400 °C, the material is 316L stainless steel, and it is designed with a cylindrical structure. There is a magnetic stirrer inside, and magnetic stirring is carried out through the magnetic stirrer 7 at the lower part of the high-pressure reactor 8. The insertion height of the bottom pipe (i.e., the liquid phase pipeline 30) at the bottom is 32 mm, and the discharging is carried out by gravity, and the continuous flow is stable at about 54 ml in the test cell. Before feeding at the start of the experiment, the bottom is paved with 15% hydrogen peroxide so that it just reaches the volume to flow out of the test cell.

[0133] At the top of test cell 13, there is a liquid feed port pipeline 6 and a gas phase pipeline 20, both of which are welded with 1 / 16 inches and are connected to the through-wall joint on the side wall of the high-pressure reactor through a ferrule nut by a 1 / 16-inch pipeline. At the bottom of test cell 13, there is also a liquid phase pipeline 30 for continuous discharging operation of the continuous flow. This 1 / 8-inch pipeline is connected to the through-wall joint on the side wall of the high-pressure reactor through a ferrule nut, and the discharging is carried out by gravity. Inside the center of the test cell, there is an internal thermocouple 14, on the outer wall insulation layer, there is an external thermocouple 15, and on the gas phase pipeline between the test cell and the material recovery tank, there is a pipeline pressure gauge 22 for collecting temperature and pressure, and the change curves of the temperature and pressure in the test cell are as Figure 4 shown, and the relationship curves of the temperature and concentration in the 15% hydrogen peroxide test material in the test cell with time are as Figure 3 shown.

[0134] High-pressure reactor 8

[0135] The design pressure of the high-pressure reactor 8 is 12 - 20 MPa, such as 15 MPa, the design temperature is 300 - 400 °C, such as 350 °C, the material is 316L stainless steel, it is designed with a columnar structure, the volume is 4L - 5L, and the wall thickness is 3 - 5 mm, such as 5 mm. There are openings on the side wall of the reactor for connecting the feed pipeline 6, the gas-phase pipeline 20 and the liquid-phase pipeline 30 of the internal test cell, as well as the power connection lines of the thermocouple and the heater, etc. The feed pipeline 6 outside the reactor is connected to the peristaltic pump 3 and then connected to the feed through-wall joint of the high-pressure reactor. There is a stop valve 2 on this pipeline; the gas-phase pipeline 20 outside the reactor is connected to the top of the material recovery tank 23 and then connected to the pressure equalizing through-wall joint of the high-pressure reactor and connected to the gas-phase pipeline 20 of the test cell. There are a pipeline thermocouple 21 and a pipeline pressure gauge 22 on this pipeline; the discharge through-wall joint of the high-pressure reactor 8 is connected to the liquid-phase pipeline 30 and then connected to the middle and lower part of the material recovery tank. All connections are made using standard Swagelok tube fittings. A gasket is used for sealing between the kettle cover 99 and the high-pressure reactor 8 and fastened with bolts. There is a pressure sensor connection port on the kettle cover 9 for connecting the pressure sensor 11 to collect the pressure outside the test cell inside the high-pressure reactor. A rupture disk is installed on the outer top of the high-pressure reactor to prevent overpressure of the high-pressure reactor. Specifically, it is installed above the kettle cover 99. In order to discharge the gas outside the test cell 13 inside the high-pressure reactor 8 in case of an emergency, the safety of the high-pressure reactor 8 is ensured. There is a pressure control system connection port on the kettle cover 9 of the high-pressure reactor. The pressure control device 10 can track the pressure according to the pressure outside the test cell inside the high-pressure reactor according to the pressure change in the test cell and use nitrogen compensation. The internal and external pressure difference is kept within the pressure that the test cell can withstand. Of course, the high-pressure reactor can also be equipped with a combustible and toxic gas alarm to prevent the leakage of combustible and toxic substances, and all electrical equipment is designed with explosion protection.

[0136] Feeding device

[0137] The feeding device includes a feed tank 1, a feed pipeline 6 where the feed pump 3 is connected to the liquid feed port of the test cell. In the experiment, hydrogen peroxide with a concentration of 15% is fed from the top of the test cell. The temperature on the feed pipeline 6 is controlled at 25 °C, and the feed rate of the feed pump is 2 ml / min.

[0138] Temperature control system

[0139] Set the operation mode of the automatic control system to isothermal and adiabatic mode. The first set of isothermal temperature is 50 °C. Wait for 15 min. If no heat release is detected, raise the temperature by 10 °C to 60 °C and then isothermal for 15 min, and so on. Heat release is detected when the isothermal temperature is 90 °C.

[0140] Analysis device 31

[0141] The analysis device 31 can be connected to a liquid chromatograph for detecting the hydrogen peroxide component analysis of the stream flowing out of the test cell in the continuous process and determining the conversion rate.

[0142] Of course, the analysis device can also be an analytical instrument such as a gas chromatograph, a liquid chromatograph, a mass spectrometer, etc., which is used for operations such as detecting the composition analysis of the stream flowing out of the sample pool in the continuous process, and conducting relevant determinations of the conversion rate. Due to the differences in the reaction systems, the operators and analysts can jointly determine the connected instruments and equipment as well as the processing methods, which will not be elaborated here.

[0143] Material recovery tank 23

[0144] The volume of the material recovery tank 23 is 1 - 5 L, the design pressure is 10 - 20 MPa, preferably 15 MPa, the design temperature is 300 - 400 °C, preferably 400 °C, and it is designed in a columnar structure. A pipeline thermocouple 21 is provided on the gas pipeline 20 connecting the top of the material recovery tank to the test pool 13. A flow totalizer, a three-way sampling valve 29, and a stop valve 28 are provided on the liquid pipeline 30 connecting the middle and lower parts of the material recovery tank 23 to the test pool. A drain valve 26 is provided at the bottom of the material recovery tank 23. The outside of the material recovery tank 23 and the connecting pipelines to the test pool are all wrapped with jackets, and temperature control is carried out through the jacket tracking heater 27. To prevent the situation of evaporation heat transfer due to exceeding the boiling point of water during the test, about 30 bar of nitrogen backpressure is filled into the upper spaces of the material recovery tank and the test pool before introducing the material. There is water in the test pool 13, and the backpressure can prevent the test material in the test pool 13 from boiling when it reaches 100 °C.

[0145] Through the continuous process material thermal stability adiabatic measurement system designed by the present disclosure, test experiments can be conveniently carried out, time can be saved, it has a small thermal inertia, can customize the test pool according to the actual or ideal situation to simulate the real continuous working conditions, and can be connected to the analysis equipment. Adiabatic testing can be better achieved by using pressure tracking and temperature tracking technologies. The measured data can be directly applied in engineering, which can provide reliable data for the continuous process design of chemical plants, prevent overprotection, and save a large amount of manpower and material resources.

[0146] There is no relevant research on this method in China. Compared with the small-scale experimental device VSP2 developed by the DIERS of the American Emergency Relief System Design Association, this experimental method can simulate the continuous process, and can customize the test pool for experiments according to the actual situation, and can conduct real-time analysis. Therefore, this method saves time and effort, has powerful functions, and has a small thermal inertia, and can conduct simulation experiments on the continuous process to measure the thermal stability of substances and develop technologies.

[0147] It should be noted that for the foregoing method embodiments, for the sake of simple description, they are all expressed as a series of action combinations. However, those skilled in the art should know that the present disclosure is not limited by the described action sequence, because according to the present disclosure, certain steps can be performed in other sequences or simultaneously. Secondly, those skilled in the art should also know that the embodiments described in the specification are all optional embodiments, and the actions and modules involved are not necessarily essential to the present disclosure.

[0148] The above is the introduction of the method embodiments. The following further illustrates the solution of the present disclosure through device embodiments.

[0149] Figure 5 The flowchart of the continuous adiabatic test method 500 for the thermal stability of substances according to an embodiment of the present disclosure is shown. As Figure 5 shown, the method is applicable to a continuous adiabatic test system for the thermal stability of substances. The system includes a feeding device, a high-pressure reactor, a material recovery tank, and an analysis device. A test cell is placed in the high-pressure reactor and a cell heater is wrapped outside the test cell. The feeding device, the material recovery tank, and the analysis device are all connected to the test cell. The method 500 includes:

[0150] Step 510, the feeding device provides test materials for the test cell;

[0151] Step 520, the cell heater heats the test cell so that the test materials start a chemical reaction;

[0152] Step 530, the material recovery tank recovers the reactants generated during the chemical reaction of the test materials;

[0153] Step 540, the analysis device analyzes the reactants to determine the conversion rate of the test materials.

[0154] Those skilled in the art can clearly understand that for the convenience and brevity of description, the specific working processes of the described modules can refer to the corresponding processes in the foregoing method embodiments and will not be elaborated herein.

[0155] According to an embodiment of the present disclosure, the present disclosure also provides an electronic device and a non-transitory computer-readable storage medium storing computer instructions.

[0156] Figure 6FIG. 600 is a schematic block diagram of an electronic device that can be used to implement embodiments of the present disclosure. The electronic device is intended to represent various forms of digital computers, such as, for example, laptop computers, desktop computers, workstations, personal digital assistants, servers, blade servers, mainframe computers, and other suitable computers. The electronic device may also represent various forms of mobile devices, such as, for example, personal digital processors, cellular telephones, smart phones, wearable devices, and other similar computing devices. The components shown herein, their connections and relationships, and their functions are merely exemplary and are not intended to limit the implementation of the present disclosure described and / or claimed herein.

[0157] Device 600 includes a computing unit 601 that can perform various appropriate actions and processes in accordance with a computer program stored in a read-only memory (ROM) 602 or a computer program loaded from a storage unit 608 into a random access memory (RAM) 603. In the RAM 603, various programs and data required for the operation of the device 600 can also be stored. The computing unit 601, the ROM 602, and the RAM 603 are connected to each other via a bus 604. An input / output (I / O) interface 605 is also connected to the bus 604.

[0158] A plurality of components in the device 600 are connected to the I / O interface 605, including: an input unit 606, such as a keyboard, a mouse, etc.; an output unit 607, such as various types of displays, speakers, etc.; a storage unit 608, such as a magnetic disk, an optical disk, etc.; and a communication unit 609, such as a network card, a modem, a wireless communication transceiver, etc. The communication unit 609 allows the device 600 to exchange information / data with other devices via a computer network such as the Internet and / or various telecommunication networks.

[0159] The computing unit 601 can be various general-purpose and / or special-purpose processing components with processing and computing capabilities. Some examples of the computing unit 601 include, but are not limited to, a central processing unit (CPU), a graphics processing unit (GPU), various dedicated artificial intelligence (AI) computing chips, various computing units running machine learning model algorithms, a digital signal processor (DSP), and any suitable processor, controller, microcontroller, etc. The computing unit 601 executes the various methods and processes described above, such as method 500. For example, in some embodiments, method 500 may be implemented as a computer software program tangibly embodied in a machine-readable medium, such as the storage unit 608. In some embodiments, part or all of the computer program may be loaded and / or installed onto the device 600 via the ROM 602 and / or the communication unit 609. When the computer program is loaded into the RAM 603 and executed by the computing unit 601, one or more steps of the method 500 described above can be executed. Alternatively, in other embodiments, the computing unit 601 may be configured to execute method 500 in any other suitable manner (e.g., by means of firmware).

[0160] Various embodiments of the systems and techniques described above in this document can be implemented in digital electronic circuitry, integrated circuit systems, field-programmable gate arrays (FPGA), application-specific integrated circuits (ASIC), application-specific standard products (ASSP), systems-on-chip (SOC), complex programmable logic devices (CPLD), computer hardware, firmware, software, and / or combinations thereof. These various embodiments can include: being implemented in one or more computer programs that can be executed and / or interpreted on a programmable system including at least one programmable processor, which can be a dedicated or general-purpose programmable processor that receives data and instructions from a storage system, at least one input device, and at least one output device, and transmits the data and instructions to the storage system, the at least one input device, and the at least one output device.

[0161] The program code for implementing the methods of the present disclosure can be written in any combination of one or more programming languages. These program codes can be provided to a processor or controller of a general-purpose computer, a special-purpose computer, or other programmable data processing device, such that when the program codes are executed by the processor or controller, the functions / operations specified in the flowchart and / or block diagram are implemented. The program code can be executed entirely on the machine, partially on the machine, as an independent software package partially on the machine and partially on a remote machine, or entirely on a remote machine or server.

[0162] In the context of this disclosure, a machine-readable medium can be a tangible medium that can contain or store a program for use by or in connection with an instruction execution system, apparatus, or device. A machine-readable medium can be a machine-readable signal medium or a machine-readable storage medium. A machine-readable medium can include, but is not limited to, electronic, magnetic, optical, electromagnetic, infrared, or semiconductor systems, apparatus, or devices, or any suitable combination of the foregoing. More specific examples of a machine-readable storage medium would include an electrical connection based on one or more wires, a portable computer diskette, a hard disk, a random access memory (RAM), a read-only memory (ROM), an erasable programmable read-only memory (EPROM or Flash memory), an optical fiber, a portable compact disc read-only memory (CD-ROM), an optical storage device, a magnetic storage device, or any suitable combination of the foregoing.

[0163] To provide for interaction with a user, the systems and techniques described herein can be implemented on a computer having: a display device (e.g., a CRT (cathode ray tube) or LCD (liquid crystal display) monitor) for displaying information to the user; and a keyboard and a pointing device (e.g., a mouse or a trackball) by which the user can provide input to the computer. Other kinds of devices can also be used to provide for interaction with the user; for example, feedback provided to the user can be any form of sensory feedback (e.g., visual feedback, auditory feedback, or tactile feedback); and input from the user can be received in any form (including acoustic, speech, or tactile input).

[0164] The systems and techniques described herein can be implemented in a computing system that includes back-end components (e.g., as a data server), or a computing system that includes middleware components (e.g., an application server), or a computing system that includes front-end components (e.g., a user computer having a graphical user interface or a web browser through which the user can interact with an implementation of the systems and techniques described herein), or a computing system that includes any combination of such back-end components, middleware components, or front-end components. The components of the system can be interconnected by any form or medium of digital data communication (e.g., a communication network). Examples of communication networks include: a local area network (LAN), a wide area network (WAN), and the Internet.

[0165] A computing system can include a client and a server. The client and the server are generally remote from each other and typically interact through a communication network. The client-server relationship is created by computer programs running on the respective computers and having a client-server relationship to each other. The server can be a cloud server, a server of a distributed system, or a server incorporating a blockchain.

[0166] It should be understood that the various forms of processes shown above can be used, with steps reordered, added or deleted. For example, the steps described in this disclosure can be executed in parallel, sequentially or in different orders, as long as the desired results of the technical solutions disclosed in this disclosure can be achieved, and no limitation is imposed herein.

[0167] The above specific embodiments do not constitute a limitation on the protection scope of this disclosure. Those skilled in the art should understand that various modifications, combinations, sub - combinations and substitutions can be made according to design requirements and other factors. Any modifications, equivalent substitutions and improvements made within the spirit and principles of this disclosure shall be included within the protection scope of this disclosure.

Claims

1. A continuous adiabatic test system for the thermal stability of substances, characterized in that, The system includes: a feeding device, a high-pressure reactor, a material recovery tank, and an analysis device. A test cell is placed inside the high-pressure reactor, and a cell heater is wrapped around the outside of the test cell. The feeding device, the material recovery tank, and the analysis device are all connected to the test cell. Among them: The feeding device is used to provide test materials for the test cell; The cell heater is used to heat the test cell so that the test materials start a chemical reaction; The material recovery tank is used to recover the reactants generated during the chemical reaction of the test materials; The analysis device is used to analyze the reactants to determine the conversion rate of the test materials; The system further includes: a gas pipeline and a liquid pipeline, and a temperature tracking heater. The temperature tracking heater is wrapped around the outside of the gas pipeline, the material recovery tank, and the liquid pipeline, and is used to start heating when the temperature inside the gas pipeline or the material recovery tank is lower than the temperature inside the test cell; Actually, a heat tracing device is wrapped around the outside of the gas pipeline, the material recovery tank, and the liquid pipeline, and the temperature tracking heater is wrapped around the outside of the heat tracing device and is used to heat the heat tracing device; the heat tracing device is a multi-section heat tracing belt; The system further includes: A kettle cover, a pressure connection pipeline, a pressure sensor, and a pressure control device; A gasket is used for sealing between the kettle cover and the high-pressure reactor, and bolts are used for fastening; One end of the pressure connection pipeline is connected to the kettle cover and extends into the high-pressure reactor, and the other end is connected to the pressure control device; The pressure sensor is installed on the pressure connection pipeline. The pressure sensor is used to collect the pressure outside the test cell and upload it for recording; The pressure control device, located above the kettle cover, is used to inflate or exhaust gas into the high-pressure reactor through the pressure connection pipeline according to the pressure difference between the pressure outside the test cell and the pressure inside the test cell; and The system further includes: A magnetic stirrer, which is located at the bottom of the high-pressure reactor; The magnetic stirrer cooperates with the magnetic stir bar inside the test cell to stir the test materials inside the test cell.

2. The system according to claim 1, characterized in that, The system further includes: a gas pipeline and a liquid pipeline, The gas pipeline is connected between the top of the test cell and the top of the material recovery tank, The liquid pipeline is connected between the bottom of the test cell and the middle and lower part of the material recovery tank.

3. The system according to claim 2, characterized in that, A first heat insulation layer, an external tracking heater, and a second heat insulation layer are further provided inside the high-pressure reactor, The first heat insulation layer is wrapped around the outside of the test cell, and the cell heater is arranged inside the heat insulation layer; The external tracking heater is wrapped around the outside of the first heat insulation layer and is used to heat the first heat insulation layer when the temperature of the first heat insulation layer is lower than the temperature inside the test cell; among them, both the external tracking heater and the cell heater open upward; The second heat insulation layer is located inside the high-pressure reactor and outside the external tracking heater.

4. The system according to claim 3, characterized in that, An internal thermocouple and an external thermocouple are further provided inside the high-pressure reactor. The internal thermocouple is inserted inside the test cell for measuring the temperature inside the test cell and uploading it for recording. The external thermocouple is inserted inside the first insulation layer for measuring the temperature of the first insulation layer and uploading it for recording.

5. The system according to claim 2, wherein The system further includes: a pipeline thermocouple, a pipeline pressure gauge, a gas-phase space thermocouple, and a liquid-phase space thermocouple; The pipeline thermocouple and the pipeline pressure gauge are connected to the gas pipeline at the top of the material recovery tank. The pipeline thermocouple is used for measuring the temperature on the gas pipeline and uploading it for recording. The pipeline pressure gauge is used for measuring the pressure inside the test cell and uploading it for recording. Both the gas-phase space thermocouple and the liquid-phase space thermocouple are installed inside the material recovery tank, respectively used for measuring the temperature of the gas-phase space and the liquid-phase space inside the material recovery tank and uploading it for recording.

6. The system according to claim 5, wherein The system further includes: a three-way sampling valve and a stop valve, The three-way sampling valve is installed on the liquid pipeline and connected to the analysis device. The stop valve is located at the end of the liquid pipeline, close to the material recovery tank.

7. The system according to any one of claims 1 to 6, characterized in that The feeding device includes: a feeding tank, a feeding tank bottom valve, a feeding pump, a raw material flowmeter, a heat exchanger, and a feeding pipeline; The feeding tank bottom valve is located at the bottom of the feeding tank. The feeding pump is connected to the feeding tank bottom valve and the raw material flowmeter. The heat exchanger is connected to the raw material flowmeter and the feeding pipeline. The feeding pipeline is connected to the top of the test cell.

8. A continuous adiabatic test method for the thermal stability of substances, characterized in that The method is applicable to a continuous adiabatic test system for the thermal stability of substances. The system includes a feeding device, a high-pressure reactor, a material recovery tank, and an analysis device. Inside the high-pressure reactor, there is a test cell and outside the test cell is wrapped with a cell heater. The feeding device, the material recovery tank, and the analysis device are all connected to the test cell. The method includes: The feeding device provides test materials for the test cell. The cell heater heats the test cell, causing the test materials to start a chemical reaction. The material recovery tank recovers the reactants generated during the chemical reaction of the test materials. The analysis device analyzes the reactants to determine the conversion rate of the test materials. The system further includes: a gas pipeline and a liquid pipeline, a temperature tracking heater. The temperature tracking heater is wrapped around the periphery of the gas pipeline, the material recovery tank, and the liquid pipeline, and is turned on for heating when the temperature inside the gas pipeline or the material recovery tank is lower than the temperature inside the test cell. Among them, What is actually wrapped around the periphery of the gas pipeline, the material recovery tank, and the liquid pipeline is a heat tracing device, and the temperature tracking heater is wrapped around the periphery of the heat tracing device to heat the heat tracing device. The heat tracing device is a multi-section heat tracing belt. The system further includes: a kettle cover, a pressure connection pipeline, a pressure sensor, and a pressure control device; A gasket is used for sealing between the kettle cover and the high-pressure reactor, and bolts are used for fastening. One end of the pressure connection pipeline is connected to the kettle cover and extends into the high-pressure reactor, and the other end is connected to the pressure control device. The pressure sensor is installed on the pressure connection pipeline, and the pressure sensor is used to collect the pressure outside the test cell and upload it for recording; The pressure control device, located above the kettle cover, inflates or exhausts the high-pressure reactor through the pressure connection pipeline according to the pressure difference between the pressure outside the test cell and the pressure inside the test cell; and The system further includes: A magnetic stirrer, which is located at the bottom of the high-pressure reactor; The magnetic stirrer cooperates with the magnetic stirrer in the test cell to stir the test material in the test cell.

9. An electronic device, characterized in that, Comprising: At least one processor; And A memory communicatively connected to the at least one processor; wherein, The memory stores instructions executable by the at least one processor, and the instructions are executed by the at least one processor so that the at least one processor can execute the method recited in claim 8.

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