Method, device and equipment for obtaining thermal correction coefficient of intermittent device
By measuring the temperature rise parameters of intermittent equipment under isothermal and adiabatic conditions and calculating the thermal correction coefficient using the thermal balance formula, the problem of the inability to accurately assess the risk of thermal runaway in existing technologies is solved, and a precise assessment of the degree of risk of thermal runaway is achieved.
Patent Information
- Application Number
- CN202311061868.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-22
- Publication Date
- 2026-08-25
- Estimated Expiration
- 2043-08-22
AI Technical Summary
Existing technologies cannot accurately measure the thermal correction factor of intermittent equipment, making it impossible to effectively assess the degree of risk of thermal runaway.
By controlling a fully automatic reaction calorimeter to measure the theoretical and actual adiabatic temperature rise, specific heat capacity, and equipment parameters of materials in intermittent equipment under isothermal and adiabatic modes, the thermal correction coefficient is calculated using the heat balance formula.
It enables accurate assessment of the risk of thermal runaway in intermittent equipment and provides precise safety assessment methods.
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Figure CN117054477B_ABST
Abstract
Description
Technical Field
[0001] This disclosure relates to the field of chemical reaction safety analysis and assessment, and in particular to the field of obtaining thermal correction coefficients for intermittent equipment. Background Technology
[0002] Currently, with social development, chemical safety production has increasingly attracted people's attention, and thermal runaway is a major cause of chemical safety accidents. When thermal runaway occurs, whether it originates from the target reaction or a secondary decomposition reaction, a large amount of heat is generated in a short period of time. The rate of heat generation is far greater than the rate of heat dissipation, making this process approximate an adiabatic process. A very important factor in assessing the degree of danger of thermal runaway is the thermal correction factor (also known as the thermal inertia factor, phi value, φ). The thermal correction factor is the ratio of the total heat capacity of the container and materials to the heat capacity of the materials. Thus, when the thermal correction factor is 1, it means that when the thermal reaction inside the equipment runs away, the total heat capacity of the container is zero, that is, the equipment wall does not absorb any heat. Therefore, thermal runaway is most dangerous when the thermal correction factor is 1. When the thermal correction factor is greater than 1, it means that when the thermal reaction inside the equipment runs away, the total heat capacity of the container is not zero, and the larger the thermal correction factor, the more heat is absorbed by the equipment wall. Therefore, the degree of danger of thermal runaway is lower in this case.
[0003] However, there is no accurate method in the industry to measure the thermal correction factor, thus making it impossible to accurately measure the degree of danger of thermal runaway. Summary of the Invention
[0004] This disclosure provides a method, apparatus, device, and storage medium for obtaining the thermal correction coefficient of intermittent equipment.
[0005] According to a first aspect of this disclosure, a method for obtaining the thermal correction factor of an intermittent device is provided. The method includes:
[0006] During the chemical reaction in the intermittent equipment, the fully automatic reaction calorimeter is controlled to operate in isothermal mode to measure the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops. The intermittent equipment is located inside the fully automatic reaction calorimeter and is the reaction vessel controlled by the fully automatic reaction calorimeter. In the isothermal mode, the fully automatic reaction calorimeter controls the temperature of the material in the intermittent equipment to remain constant.
[0007] During the chemical reaction in the intermittent equipment, the fully automatic reaction calorimeter is controlled to operate in adiabatic mode to obtain the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops. In the adiabatic mode, the temperature of the jacket wrapped around the outer wall of the intermittent equipment is controlled by the fully automatic reaction calorimeter to change synchronously with the material temperature. The equipment parameters are related to the heat transfer coefficient and heat transfer area of the intermittent equipment.
[0008] Based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment, the thermal correction coefficient of the intermittent equipment is obtained.
[0009] In addition to the aspects and any possible implementations described above, a further implementation is provided in which the measurement of the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops includes:
[0010] The exothermic enthalpy and specific heat capacity of the intermittent equipment are obtained by measuring the fully automated reaction calorimeter.
[0011] Obtain the initial total mass of materials added to the intermittent equipment;
[0012] The theoretical adiabatic temperature rise is calculated based on the exothermic enthalpy, the specific heat capacity, and the initial total mass of the material.
[0013] In addition to the aspects and any possible implementations described above, a further implementation is provided in which the fully automatic reaction calorimeter is controlled to operate in adiabatic mode, comprising:
[0014] According to the preset temperature rise step, the material temperature in the intermittent equipment is gradually increased, and the jacket temperature corresponding to the material temperature is calculated simultaneously to synchronously control the jacket temperature.
[0015] In addition to the aspects and any possible implementations described above, a further implementation is provided in which the calculation of the jacket temperature corresponding to the material temperature includes:
[0016] Obtain a pre-stored adiabatic temperature relationship between the material temperature and the jacket temperature, wherein the adiabatic temperature relationship is determined based on at least one of the following: the type of the intermittent equipment, the type of material, and the temperature difference between the jacket temperature and the material temperature.
[0017] Based on the material temperature inside the intermittent equipment and the adiabatic temperature relationship, the jacket temperature corresponding to the material temperature is calculated.
[0018] In addition to the aspects and any possible implementations described above, a further implementation is provided in which the device parameters of the intermittent device are obtained through the following steps:
[0019] After the chemical reaction stops, while keeping the material temperature constant, the heating device is controlled to perform a first heating operation on the material in the intermittent equipment, and the heating heat used in the first heating operation is obtained;
[0020] The first temperature difference between the jacket and the material is obtained when the temperature of the jacket stops changing under the heating heat and the heat absorption of the jacket.
[0021] The equipment parameters are calculated based on the heating heat and the first temperature difference.
[0022] In addition to the aspects and any possible implementations described above, a further implementation is provided in which the specific heat capacity of the material is obtained through the following steps:
[0023] After calculating the equipment parameters, the heating device is controlled to perform a second heating operation on the material in the intermittent equipment, and heating is stopped when the temperature rise of the material reaches the preset temperature rise.
[0024] Under the second heating operation, obtain the second temperature difference between the jacket and the material, and the heating rate of the material in the intermittent device;
[0025] The specific heat capacity of the material is calculated based on the equipment parameters, the second temperature difference, the mass of the material in the intermittent equipment, and the material heating rate.
[0026] In addition to the aspects and any possible implementations described above, a further implementation is provided, wherein obtaining the thermal correction coefficient of the intermittent equipment based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment includes:
[0027] Based on the preset heat balance formula for material reaction, a curve showing the relationship between thermal time parameters, reaction time, and temperature difference between the jacket and the material is obtained. The thermal time parameter is a function of the thermal correction coefficient, the total initial mass of material added to the intermittent equipment, the specific heat capacity of the material, and the equipment parameters.
[0028] The thermal time parameter is obtained by processing the relationship curve.
[0029] The thermal correction factor of the intermittent equipment is calculated based on the thermal time parameter, the theoretical adiabatic temperature rise, and the actual adiabatic temperature rise.
[0030] In addition to the aspects and any possible implementations described above, a further implementation is provided in which the calculation of the thermal correction coefficient of the intermittent equipment based on the thermal time parameter, the theoretical adiabatic temperature rise, and the actual adiabatic temperature rise includes:
[0031] The theoretical thermal correction coefficient is calculated based on the thermal time parameter, the initial total mass of the material, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment.
[0032] Calculate the actual thermal correction factor based on the theoretical adiabatic temperature rise and the actual adiabatic temperature rise;
[0033] The theoretical thermal correction factor is verified based on the actual thermal correction factor. If the verification passes, the theoretical thermal correction factor is taken as the final thermal correction factor.
[0034] According to a second aspect of this disclosure, a device for obtaining the thermal correction coefficient of an intermittent device is provided. The device includes:
[0035] The first processing module is used to control the fully automatic reaction calorimeter to operate in isothermal mode during the chemical reaction in the intermittent equipment, so as to measure the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops. The intermittent equipment is located inside the fully automatic reaction calorimeter and is the reaction vessel to be controlled by the fully automatic reaction calorimeter. In the isothermal mode, the fully automatic reaction calorimeter controls the temperature of the material in the intermittent equipment to remain constant.
[0036] The second processing module is used to control the fully automatic reaction calorimeter to operate in adiabatic mode during the chemical reaction in the intermittent equipment, and to obtain the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops. In the adiabatic mode, the fully automatic reaction calorimeter controls the temperature of the jacket wrapped around the outer wall of the intermittent equipment to change synchronously with the material temperature. The equipment parameters are related to the heat transfer coefficient and heat transfer area of the intermittent equipment.
[0037] The acquisition module is used to acquire the thermal correction coefficient of the intermittent equipment based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment.
[0038] According to a third aspect of this disclosure, an electronic device is provided. The electronic device includes a memory and a processor, wherein the memory stores a computer program, and the processor executes the program to implement the method described above.
[0039] According to a fourth aspect of this disclosure, a computer-readable storage medium is provided having a computer program stored thereon that, when executed by a processor, implements the methods according to the first and / or second aspects of this disclosure.
[0040] In this disclosure, during the chemical reaction in the intermittent equipment, by controlling the fully automatic reaction calorimeter to operate in isothermal mode, the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops can be automatically measured. Then, during the chemical reaction in the intermittent equipment, the fully automatic reaction calorimeter is controlled to operate in adiabatic mode to obtain the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops. Subsequently, based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment, the thermal correction coefficient of the intermittent equipment can be accurately obtained, thereby facilitating the accurate assessment of the degree of risk of thermal reaction runaway.
[0041] It should be understood that the description in the Summary of the Invention is not intended to limit the key or essential features of the embodiments of this disclosure, nor is it intended to restrict the scope of this disclosure. Other features of this disclosure will become readily apparent from the following description. Attached Figure Description
[0042] The above and other features, advantages, and aspects of the embodiments of this disclosure will become more apparent from the accompanying drawings and the following detailed description. The drawings are provided for a better understanding of the invention and are not intended to limit the scope of this disclosure. In the drawings, the same or similar reference numerals denote the same or similar elements, wherein:
[0043] Figure 1 A flowchart is shown of a method for obtaining the thermal correction coefficient of an intermittent device according to an embodiment of the present disclosure;
[0044] Figure 2 A test curve of a fully automated reaction calorimeter according to an embodiment of the present disclosure is shown;
[0045] Figure 3 Another fully automated reaction calorimeter test curve according to an embodiment of the present disclosure is shown;
[0046] Figure 4 A block diagram of a system for obtaining the thermal correction coefficient of an intermittent device according to an embodiment of the present disclosure is shown;
[0047] Figure 5 A block diagram of a device for obtaining the thermal correction coefficient of an intermittent device according to an embodiment of the present disclosure is shown;
[0048] Figure 6 A block diagram of an exemplary electronic device capable of implementing embodiments of the present disclosure is shown. Detailed Implementation
[0049] To make the objectives, technical solutions, and advantages of the embodiments of this disclosure clearer, the technical solutions of the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this disclosure, and not all embodiments. Based on the embodiments of this disclosure, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this disclosure.
[0050] Furthermore, the term "and / or" in this article is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. Additionally, the character " / " in this article generally indicates that the preceding and following related objects have an "or" relationship.
[0051] Figure 1 A flowchart of a method 100 for obtaining the thermal correction factor of an intermittent device according to an embodiment of the present disclosure is shown. Method 100 may include:
[0052] Step 110: During the chemical reaction in the intermittent equipment, the fully automatic reaction calorimeter is controlled to operate in isothermal mode to measure the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops. The intermittent equipment is located inside the fully automatic reaction calorimeter and is the reaction vessel controlled by the fully automatic reaction calorimeter. In the isothermal mode, the fully automatic reaction calorimeter controls the temperature of the material in the intermittent equipment to remain constant.
[0053] Intermittent equipment can include intermittent reactors, which are devices that carry out chemical reactions intermittently.
[0054] Fully automated reaction calorimeters can include RC1 (Reaction Calorimeter) or RC HP-1000 and other reaction calorimeters from different manufacturers. These calorimeters are used to measure the heat released or absorbed in a chemical reaction. They are primarily used to evaluate the thermal effects of chemical reactions, providing data support for the safe operation of the reaction. They typically consist of a batch reactor of varying sizes (i.e., the aforementioned intermittent equipment), a temperature control module, and control software, within which key process parameters related to the reaction are accurately monitored.
[0055] like Figure 4 As shown, the fully automatic reaction calorimeter includes an intermittent device and a control box. The computer, through the control box, can control the fully automatic reaction calorimeter to operate in different modes. In turn, the fully automatic reaction calorimeter can perform different controls on the intermittent device in different modes. Specifically, it can control the fully automatic reaction calorimeter to operate in isothermal mode, adiabatic mode, and constant temperature mode.
[0056] In isothermal mode, the fully automatic reaction calorimeter controls the material temperature inside the intermittent equipment to remain constant;
[0057] In adiabatic mode, the fully automatic reaction calorimeter controls the temperature of the jacket wrapped around the outer wall of the intermittent equipment to change synchronously with the material temperature. That is, when the material temperature rises, the jacket temperature rises, and when the material temperature falls, the jacket temperature falls. The purpose is to ensure that the temperature of the jacket is as similar as possible to the material temperature.
[0058] In constant temperature mode, the fully automatic reaction calorimeter controls the temperature of the jacket wrapped around the outer wall of the intermittent equipment to remain constant.
[0059] The jacket surrounding the outer wall of the intermittent equipment is wrapped around the perimeter and bottom of the intermittent equipment. The jacket contains flowing cold oil or other heat exchanger. The intermittent equipment can be heated or cooled by adjusting the temperature of the heat exchanger inside the jacket.
[0060] in addition, Figure 4 The feed pump in the middle can pump the material in the feed container into the intermittent equipment, so that the intermittent equipment can use the material to carry out chemical reactions.
[0061] Step 120: During the chemical reaction in the intermittent equipment, the fully automatic reaction calorimeter is controlled to operate in adiabatic mode to obtain the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops. In the adiabatic mode, the temperature of the jacket wrapped around the outer wall of the intermittent equipment is controlled to change synchronously with the material temperature. The equipment parameters are related to the heat transfer coefficient and heat transfer area of the intermittent equipment. Specifically, the equipment parameters can be the product of the heat transfer coefficient and heat transfer area of the intermittent equipment.
[0062] The chemical reaction in step 120 is exactly the same as that in step 110. The materials used and the amounts of materials are the same, and both are from the beginning to the end of the chemical reaction. The only difference is that the working mode of the fully automatic reaction calorimeter is different, so that different parameters can be effectively measured during the chemical reaction process in the intermittent equipment.
[0063] Step 130: Obtain the thermal correction coefficient of the intermittent equipment based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment.
[0064] During the chemical reaction in the intermittent equipment, by controlling the fully automatic reaction calorimeter to operate in isothermal mode, the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops can be automatically measured. Then, during the chemical reaction in the intermittent equipment, by controlling the fully automatic reaction calorimeter to operate in adiabatic mode, the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops can be obtained. Subsequently, based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment, the thermal correction coefficient of the intermittent equipment can be accurately obtained, thereby facilitating the accurate assessment of the degree of risk of thermal reaction runaway.
[0065] For example, if it is determined through other means that the ideal adiabatic temperature rise of the intermittent equipment is 100 degrees when the thermal reaction inside the intermittent equipment runs out of control, then when the thermal correction factor is 1, the ideal adiabatic temperature rise of the intermittent equipment can be determined to be 100℃; when the thermal correction factor is 2, the ideal adiabatic temperature rise of the intermittent equipment can be determined to be 50℃ instead of 100℃; when the thermal correction factor is 4, the ideal adiabatic temperature rise of the intermittent equipment can be determined to be 25℃; and even the temperature rise time corresponding to the theoretical adiabatic temperature rise can be determined, thereby accurately quantifying the degree of danger of thermal reaction runaway.
[0066] In some embodiments, measuring the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops includes:
[0067] The exothermic enthalpy and specific heat capacity of the intermittent equipment are obtained by measuring the fully automated reaction calorimeter.
[0068] Exothermic enthalpy is the enthalpy change of a reaction, which is the heat released or absorbed during a chemical reaction.
[0069] Specific heat capacity, denoted by the symbol c, is the heat capacity per unit mass of a substance, that is, the amount of heat absorbed or released when a unit mass of an object changes temperature by a unit amount.
[0070] Obtain the initial total mass of materials added to the intermittent equipment;
[0071] The initial total mass of materials is the sum of the masses of all materials added to the batch equipment during the chemical reaction process. The materials added to the batch equipment can be materials added all at once or materials added in batches. In short, it is the sum of the masses of all materials added for the chemical reaction process.
[0072] The theoretical adiabatic temperature rise is calculated based on the exothermic enthalpy, the specific heat capacity, and the initial total mass of the material.
[0073] By acquiring the exothermic enthalpy and specific heat capacity of the intermittent equipment measured by a fully automatic reaction calorimeter, as well as the total mass of the initial material added to the intermittent equipment, the theoretical adiabatic temperature rise can be automatically calculated based on the exothermic enthalpy, specific heat capacity, and total mass of the initial material. That is, theoretical adiabatic temperature rise = exothermic enthalpy / specific heat capacity / total mass of initial material.
[0074] To measure the exothermic enthalpy and theoretical adiabatic temperature rise of the acetic anhydride hydrolysis reaction using the RC1mx isothermal mode: Add approximately 862g of water to the reactor (batch reactor), use an anchor paddle, operate at 150rpm, and program the temperature to 22℃. After the temperature reaches 22℃ and stabilizes for 30 minutes, begin pre-calibration (i.e., the standard calibration performed before adding acetic anhydride in isothermal mode is called pre-calibration). After pre-calibration, maintain the temperature at 25℃ and add approximately 158g of acetic anhydride dropwise at a rate of 20g / min using a pump. After the addition is complete, continue the reaction at 25℃ for approximately 1 hour. After the reaction is complete, begin post-calibration. Processing the experimental data yields an exothermic enthalpy of 87.0KJ and a theoretical adiabatic temperature rise of 21.9℃. The total heat of the initial material = 862g + 158g = 1020g. The theoretical adiabatic temperature rise = exothermic enthalpy measured by RC1 / specific heat capacity measured by RC1 / total mass of the initial material 1020g.
[0075] In some embodiments, controlling the fully automatic reaction calorimeter to operate in adiabatic mode includes:
[0076] According to the preset temperature rise step, the material temperature in the intermittent equipment is gradually increased, and the jacket temperature corresponding to the material temperature is calculated simultaneously to synchronously control the jacket temperature.
[0077] The initial temperature and preset temperature rise step of the material in the intermittent equipment can be customized. Then, based on the initial temperature, the material temperature in the intermittent equipment is gradually increased according to the preset temperature rise step. For example, the initial situation is to control the material to be calibrated isothermally at 25°C and wait for 30 minutes, and then raise the temperature by 5°C at a rate of 1K / min and wait for 30 minutes. At the same time, for each material temperature calculated, the jacket temperature corresponding to that material temperature is calculated, that is, the jacket temperature matched with that material temperature, so that the jacket temperature is synchronously controlled, so that the jacket temperature changes as synchronously as possible with the material temperature, and ensures that the jacket temperature and the material temperature are as similar as possible, thereby eliminating the difference between the jacket temperature and the material temperature, so that the material will not transfer heat to the jacket.
[0078] In some embodiments, calculating the jacket temperature corresponding to the material temperature includes:
[0079] Obtain a pre-stored adiabatic temperature relationship between the material temperature and the jacket temperature, wherein the adiabatic temperature relationship is determined based on at least one of the following: the type of the intermittent equipment, the type of material, and the temperature difference between the jacket temperature and the material temperature.
[0080] If the adiabatic temperature relationship is T j =T r -(-0.0006*Tr 2 +0.0235Tr-0.1605), where T j Tr represents the jacket temperature, and Tr represents the material temperature.
[0081] Of course, the above adiabatic temperature relationship is not static and can be determined based on factors such as the type of intermittent equipment, the type of material, and the temperature range of the material.
[0082] Based on the material temperature inside the intermittent equipment and the adiabatic temperature relationship, the jacket temperature corresponding to the material temperature is calculated.
[0083] By calling the pre-stored adiabatic temperature relationship between the material temperature and the jacket temperature, the jacket temperature corresponding to the material temperature can be accurately calculated based on the material temperature in the intermittent equipment and the adiabatic temperature relationship, so that the jacket temperature and the material temperature are as similar as possible. In this way, the material will not transfer heat to the jacket, thus ensuring that the fully automatic reaction calorimeter works in adiabatic mode.
[0084] In some embodiments, the device parameters of the intermittent device are obtained through the following steps:
[0085] After the chemical reaction stops, while keeping the material temperature constant, the heating device is controlled to perform a first heating operation on the material in the intermittent equipment, and the heating heat used in the first heating operation is obtained;
[0086] The sign that a chemical reaction has stopped is that the material in the intermittent equipment stops releasing and absorbing heat, that is, the heat exchange has stopped.
[0087] Heating devices are those other than intermittent equipment, such as heating rods.
[0088] Maintaining a constant material temperature is to accurately obtain the heat of reaction, while controlling the heating device to perform the first heating operation on the material in the intermittent equipment is to measure the equipment parameters. The specific operation can be as follows: the heating rod continuously inputs heat with a constant power for 15 minutes, while the jacket uses the internal heat exchanger to absorb the heat until the jacket stops absorbing heat (i.e. the jacket temperature stops changing). The temperature of the jacket and the temperature of the material are then obtained, and the difference is calculated to obtain the first temperature difference between the jacket and the material.
[0089] The first temperature difference between the jacket and the material is obtained when the temperature of the jacket stops changing under the heating heat and the heat absorption of the jacket.
[0090] During the first heating operation, it is necessary to ensure that the material temperature remains constant. Therefore, the jacket is used to absorb the heating heat at this time. In theory, it will absorb all the heating heat, but in reality, due to the fact that the jacket wall also absorbs some heat or the airtightness of the intermittent equipment causes a certain amount of heat exchange, it will actually absorb some of the heating heat.
[0091] The equipment parameters are calculated based on the heating heat and the first temperature difference.
[0092] After the chemical reaction stops, while keeping the material temperature constant, the heating device is controlled to perform a first heating operation on the material in the intermittent equipment, and the heating heat used in the first heating operation is obtained. Under the heating heat and the heat absorption of the jacket, the first temperature difference between the jacket and the material is obtained when the temperature of the jacket stops changing (i.e., stops absorbing heat). Then, the equipment parameters can be accurately calculated by dividing the heating heat and the first temperature difference.
[0093] For example: A heating rod continuously supplies heat at a constant power for 15 minutes, while the jacket removes the heat. When the jacket temperature stabilizes and stops changing, the steady-state temperature difference (T) between the jacket and the material is obtained. r -T j Then divide the amount of heat generated by the first temperature difference (T) r -T j ) = UA (equipment parameters), where U is the heat transfer coefficient and A is the heat transfer area.
[0094] In some embodiments, the specific heat capacity of the material is obtained through the following steps:
[0095] After calculating the equipment parameters, the heating device is controlled to perform a second heating operation on the material in the intermittent equipment, and heating is stopped when the temperature rise of the material reaches the preset temperature rise.
[0096] The preset temperature rise can be 3℃, 5℃, etc.
[0097] After calculating the equipment parameters, the heating device can be controlled to perform a second heating operation on the material in the intermittent equipment, so that the material temperature increases by 3 degrees to achieve the preset temperature rise.
[0098] Under the second heating operation, obtain the second temperature difference between the jacket and the material, and the heating rate of the material in the intermittent device;
[0099] The duration of the process by which the material's temperature rises to the preset temperature rise is obtained, and then the material's heating rate is equal to the preset temperature rise divided by the duration.
[0100] The specific heat capacity of the material is calculated based on the equipment parameters, the second temperature difference, the mass of the material in the intermittent equipment, and the material heating rate.
[0101] Under the second heating operation, the second temperature difference between the jacket and the material, and the material heating rate within the intermittent device, are obtained. Then, based on the second heating heat, the second temperature difference, the mass of the material within the intermittent device, and the material heating rate, the specific heat capacity of the material can be automatically and accurately calculated. Specifically: UA*(T r -T j = Mass of material after chemical reaction * Specific heat capacity of material Cp,s * Heating rate of material, where the second temperature difference = (T r -T j ), where the jacket temperature is T j The material temperature is T. r .
[0102] In addition, when calculating the specific heat capacity of a material, since the material temperature increases and the equipment parameters are temperature-dependent, the equipment parameters calculated using the first heating operation may become inaccurate after the material temperature changes. Therefore, a third heating operation (exactly the same as the first heating operation) can be performed after the second heating operation to maintain the isothermal mode. Then, the steps for calculating the equipment parameters under the first heating operation are repeated to recalculate the equipment parameters to ensure their accuracy. The newly calculated equipment parameters are then used as the final equipment parameters. Of course, the newly calculated equipment parameters are no longer used to calculate the specific heat capacity of the material.
[0103] In some embodiments, obtaining the thermal correction coefficient of the intermittent equipment based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment includes:
[0104] Based on the preset heat balance formula for material reaction, a curve showing the relationship between thermal time parameters, reaction time, and temperature difference between the jacket and the material is obtained. The thermal time parameter is a function of the thermal correction coefficient, the total initial mass of material added to the intermittent equipment, the specific heat capacity of the material, and the equipment parameters.
[0105] The preset heat balance formula for the material reaction is a heat balance formula established by the fully automatic reaction calorimeter in constant temperature mode (i.e., the temperature of the jacket surrounding the intermittent equipment is kept constant by the fully automatic reaction calorimeter). The preset heat balance formula for the material reaction is as follows:
[0106] in, M is the thermal correction factor. r C represents the initial total mass of the material. p,s T represents the specific heat capacity of the material. j T represents the temperature of the jacket. r The temperature of the material is UA, and UA is the equipment parameter (where U is the heat transfer coefficient, unit: W / K / m). 2 A represents the heat transfer area, in m². 2 ), where t is time.
[0107] Thermal time parameters
[0108] In the above formula, the left side The first digit represents the power required to overcome internal energy and increase the temperature of the material during heating and cooling. The second digit represents the power input from the jacket to the material or the power output from the material to the jacket. Integrating the above formula over time t yields the heat formula.
[0109] The relationship curve diagram is as follows:
[0110] The thermal time parameter is obtained by processing the relationship curve.
[0111] The thermal correction factor of the intermittent equipment is calculated based on the thermal time parameter, the theoretical adiabatic temperature rise, and the actual adiabatic temperature rise.
[0112] By performing various processing operations such as integral calculations and logarithmic calculations on the preset material reaction heat balance formula, a relationship curve can be obtained between the thermal time parameter, reaction time, and the temperature difference between the jacket and the material. Then, by fitting this relationship curve, the slope of the processed curve can be obtained. The negative reciprocal of this slope with respect to the thermal time parameter is... Then the thermal time parameter can be obtained, and based on the thermal time parameter, the theoretical adiabatic temperature rise, and the actual adiabatic temperature rise, the thermal correction factor of the intermittent equipment can be accurately calculated.
[0113] In some embodiments, calculating the thermal correction factor for the intermittent equipment based on the thermal time parameter, the theoretical adiabatic temperature rise, and the actual adiabatic temperature rise includes:
[0114] The theoretical thermal correction coefficient is calculated based on the thermal time parameter, the initial total mass of the material, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment.
[0115] That is, calculate τ c (unit: seconds), due to thus, M r C is the initial total mass of the material.p,s UA represents the specific heat capacity of the material and the equipment parameter.
[0116] Calculate the actual thermal correction factor based on the theoretical adiabatic temperature rise and the actual adiabatic temperature rise;
[0117] The theoretical thermal correction factor is verified based on the actual thermal correction factor. If the verification passes, the theoretical thermal correction factor is taken as the final thermal correction factor.
[0118] Since the thermal time parameter is a function of the thermal correction coefficient, the initial total mass of material added to the intermittent equipment, the specific heat capacity of the material, and the equipment parameters, after determining the thermal time parameter, the theoretical thermal correction coefficient can be calculated because the initial total mass of material added to the intermittent equipment, the specific heat capacity of the material, and the equipment parameters are also determined. However, this theoretical thermal correction coefficient may not be very accurate. Therefore, the actual thermal correction coefficient can be calculated based on the theoretical adiabatic temperature rise and the actual adiabatic temperature rise. Then, the theoretical thermal correction coefficient can be cross-checked with the actual thermal correction coefficient to determine whether the theoretical thermal correction coefficient is accurate. If the check passes, it means that the theoretical thermal correction coefficient is correct. Therefore, the theoretical thermal correction coefficient can be used as the final thermal correction coefficient.
[0119] Specifically, the theoretical thermal correction factor is φ 理论真实 The actual thermal correction factor is φ 绝热 Then the relative error = |φ 绝热 -φ 理论真实 )︱ / φ 理论真实 If the relative error is less than 5% (preset error), then the theoretical thermal correction coefficient is considered to be correct; otherwise, it indicates that the theoretical thermal correction coefficient is not quite correct, and therefore, the theoretical thermal correction coefficient can be recalculated.
[0120] The technical solution of this disclosure will be further explained in detail below:
[0121] Example 1
[0122] The specific steps for obtaining and verifying the thermal correction coefficient for intermittent equipment are as follows:
[0123] (1) The exothermic enthalpy and theoretical adiabatic temperature rise of the acetic anhydride hydrolysis reaction were measured using the RC1mx isothermal mode: Approximately 698.8 g of deionized water was added to the reactor. An anchor paddle was used, and the temperature was controlled at 150 rpm with a programmed temperature control up to 25 °C. After the temperature reached 22 °C and stabilized for 30 min, pre-calibration was initiated. After pre-calibration, approximately 168.0 g of acetic anhydride was added dropwise at a rate of 20 g / min using a pump. After the addition was completed, the reaction was continued at 25 °C for approximately 1 h. After the reaction was completed, post-calibration (i.e., isothermal mode, the standard calibration performed after the reaction is called post-calibration) was initiated. The data obtained from the experiment were processed to obtain an exothermic enthalpy of 92.3 KJ and a theoretical adiabatic temperature rise of 28.7 °C. The total initial mass of the material = 698.8 g + 168.0 g = 866.8 g.
[0124] (Exothermic enthalpy measured by RC1) / (Specific heat capacity measured by RC1) (i.e., specific heat capacity of the material C) p,s The theoretical adiabatic temperature rise is calculated as follows: (1) / (Total mass of substances added to the container (Initial total mass of materials)) = Theoretical adiabatic temperature rise.
[0125] (2) Control RC1 to operate in isothermal mode. Specifically, control the material to wait at an initial temperature of 25℃ for 30 minutes, then increase the temperature by 5℃ at a rate of 1K / min (preset temperature rise step), and wait for 30 minutes. Increase the temperature in 5℃ increments until it reaches 50℃ (where the final temperature depends on the initial temperature plus the theoretical adiabatic temperature rise), and obtain the jacket temperature T of the reaction at this temperature range. j That is, T j =T r -(-0.0006*Tr 2 +0.0235Tr-0.1605 (i.e., adiabatic temperature relationship), where Tr is the material temperature. Material temperature = initial temperature + preset temperature step size * i, where i is the number of heating cycles. For example, if the initial temperature is 25℃ and the preset temperature step size is 5℃, then the material temperature after the first heating cycle is 30℃, the material temperature after the second heating cycle is 35℃, and the material temperature after the third heating cycle is 40℃.
[0126] (3) The actual adiabatic temperature rise of the acetic anhydride hydrolysis reaction was tested using the RC1mx adiabatic mode. After the reaction was completed, standard calibration was performed, and the actual adiabatic temperature rise was found to be 25.8℃. p,s The value is 3.85 J / (g·℃) and UA is 7.11 W / K.
[0127] The standard calibration refers to: waiting in isothermal mode for xx minutes, inputting constant power to the heating rod for xx minutes, while the jacket cools down to maintain the material temperature, so as to obtain the equipment parameter UA through the constant energy, heat exchange area, and temperature difference between the jacket and the material during the heating process.
[0128] Then, a constant temperature mode was adopted, and the jacket temperature was reduced to 35°C at the maximum rate and then kept constant until the material temperature remained constant. The calorimetric curve is shown below. Figure 2 As shown.
[0129] (4) When using the constant temperature mode, the thermal equilibrium inside the reactor is:
[0130] (i.e., the pre-defined heat balance formula for the material reaction)
[0131] ΔT=T j -T r →d(ΔT)=-dT r
[0132]
[0133] Make thermal time parameter Combining the above equations, we get
[0134]
[0135] in, M is the thermal correction factor. r C represents the initial total mass of the material. p,s T represents the specific heat capacity of the material. j T represents the temperature of the jacket. r The temperature of the material is UA, and UA is the equipment parameter (where U is the heat transfer coefficient, unit: W / K / m). 2 A represents the heat transfer area, in m². 2 ), where t is the unit of seconds.
[0136] Initial conditions:
[0137]
[0138] The integral yields:
[0139]
[0140] Take the logarithm:
[0141]
[0142] (5) Set the temperature T of the acetic anhydride hydrolysis reaction solution in the reactor to T r and jacket temperature T j Plotting the natural logarithm of the temperature difference as a function of time, the slope is τ. c The negative reciprocal of τ. That is, ln(ΔT / ΔT0) = -0.0019t + 0.0122, τ c = 530 seconds;
[0143] according to Obtain the φ of the intermittent device 理论真实 ,Right now
[0144] (6) By comparing the theoretical adiabatic temperature rise with the actual adiabatic temperature rise, the equipment φ can be obtained. 绝热 , i.e. φ 绝热 =Theoretical adiabatic temperature rise / Measured adiabatic temperature rise = 28.7 / 25.8 = 1.11;
[0145] (7) Compare the φ values obtained in steps (5) and (6), and the relative error is ︱φ 绝热 -φ 理论真实 )︱ / φ 理论真实 = |1.11-1.12| / 1.12 = 0.89% < 5%, so the method for obtaining the thermal correction coefficient (φ value) of intermittent equipment can be considered feasible and relatively accurate.
[0146] Example 2
[0147] The specific steps for obtaining and verifying the thermal correction coefficient for intermittent equipment are as follows:
[0148] (1) The exothermic enthalpy and theoretical adiabatic temperature rise of the acetic anhydride hydrolysis reaction were measured using the RC1mx isothermal mode: about 862g of water was added to the reactor, and the anchor paddle was used at 150rpm. The temperature was controlled to 22℃. After the temperature reached 22℃ and stabilized for 30min, the pre-calibration was started. After the pre-calibration was completed, about 158g of acetic anhydride was added dropwise at a rate of 20g / min using a pump. After the addition was completed, the reaction was continued at 25℃ for about 1h. After the reaction was completed, the post-calibration was started. The exothermic enthalpy was 87.0KJ and the theoretical adiabatic temperature rise was 21.9℃. The initial total mass of the material was 862g + 158g = 1020g.
[0149] (Exothermic enthalpy measured by RC1) / (Specific heat capacity measured by RC1) (i.e., specific heat capacity of the material C) p,s The theoretical adiabatic temperature rise is calculated as follows: (1) / (Total mass of substances added to the container (Initial total mass of materials)) = Theoretical adiabatic temperature rise.
[0150] (2) Using the reaction solution after the reaction as a standard solution, the heat loss coefficient required for the adiabatic mode was calibrated. The reaction temperature was selected as the starting temperature, and an isothermal mode was adopted. The temperature was held at 25℃ for 30 min, and then increased by 5℃ at a rate of 1K / min, and held for 30 min. The temperature was increased in increments of 5℃, eventually reaching 45℃, and the jacket temperature T of the reaction at this temperature range was obtained. j That is, Tj = Tr - (-0.0003 * Tr 2 -0.003Tr+0.3325 (i.e., the adiabatic temperature relationship), where Tr is the material temperature;
[0151] (3) The actual adiabatic temperature rise of the acetic anhydride hydrolysis reaction was tested using the RC1mx adiabatic mode. After the reaction was completed, standard calibration was performed, and the actual adiabatic temperature rise was 17.9℃, Cp,s was 3.89J / (g·℃) and UA was 10.97W / K.
[0152] Then, using a constant temperature mode, the jacket temperature was reduced to 30°C at the maximum rate and then kept constant until the sample temperature remained constant. The calorimetric curve is shown below. Figure 3 As shown;
[0153] (4) When using the constant temperature mode, the thermal equilibrium inside the reactor is:
[0154] (i.e., the pre-defined heat balance formula for the material reaction)
[0155] ΔT=T j -T r →d(ΔT)=-dT r
[0156]
[0157] make Combining the above equations, we get
[0158]
[0159] Initial conditions:
[0160]
[0161] The integral yields:
[0162] Among them, C′ p =C p,s
[0163] Take the logarithm:
[0164]
[0165] (5) Plot the natural logarithm of the temperature difference between the acetic anhydride hydrolysis reaction solution and the jacket temperature in the reactor as a function of time. The slope is τ. c The negative reciprocal of τ. That is, ln(ΔT / ΔT0) = -0.0023t + 0.0538, τ c =434;
[0166] according to Obtain the φ of the intermittent device 理论真实 ,Right now
[0167] (6) By comparing the theoretical adiabatic temperature rise with the actual adiabatic temperature rise, the equipment φ can be obtained.绝热 , i.e. φ 绝热 =Theoretical adiabatic temperature rise / Measured adiabatic temperature rise = 21.9 / 17.9 = 1.22;
[0168] (7) Compare the φ values obtained in steps (5) and (6), and the relative error is ︱φ 绝热 -φ 理论真实 )︱ / φ 理论真实 =|1.22-1.20| / 1.20 = 1.67% < 5%, which can be considered as the thermal correction factor for intermittent equipment.
[0169] (φ 理论真实 The method for obtaining the data is feasible and relatively accurate.
[0170] It should be noted that, for the sake of simplicity, the foregoing method embodiments are all described as a series of actions. However, those skilled in the art should understand that this disclosure is not limited to the described order of actions, because according to this disclosure, some steps can be performed in other orders or simultaneously. Furthermore, those skilled in the art should also understand that the embodiments described in the specification are all optional embodiments, and the actions and modules involved are not necessarily essential to this disclosure.
[0171] The above is an introduction to the method embodiments. The following describes the solution described in this disclosure further through device embodiments.
[0172] Figure 5 A block diagram of a thermal correction factor acquisition device 500 for an intermittent device according to an embodiment of the present disclosure is shown. Figure 5 As shown, the device 500 includes:
[0173] The first processing module 510 is used to control the fully automatic reaction calorimeter to operate in isothermal mode during the chemical reaction in the intermittent equipment, so as to measure the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops. The intermittent equipment is located inside the fully automatic reaction calorimeter and is the reaction vessel to be controlled by the fully automatic reaction calorimeter. In the isothermal mode, the fully automatic reaction calorimeter controls the temperature of the material in the intermittent equipment to remain constant.
[0174] The second processing module 520 is used to control the fully automatic reaction calorimeter to work in adiabatic mode during the chemical reaction in the intermittent equipment, and to obtain the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops. In the adiabatic mode, the fully automatic reaction calorimeter controls the temperature of the jacket wrapped around the outer wall of the intermittent equipment to change synchronously with the material temperature. The equipment parameters are related to the heat transfer coefficient and heat transfer area of the intermittent equipment.
[0175] The acquisition module 530 is used to acquire the thermal correction coefficient of the intermittent equipment based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment.
[0176] Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the specific working process of the described module can be referred to the corresponding process in the foregoing method embodiments, and will not be repeated here.
[0177] According to embodiments of the present disclosure, the present disclosure also provides an electronic device and a non-transitory computer-readable storage medium storing computer instructions.
[0178] Figure 6 A schematic block diagram of an electronic device 600 that can be used to implement embodiments of the present disclosure is shown. The electronic device is intended to represent various forms of digital computers, such as 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 personal digital processors, cellular phones, smartphones, wearable devices, and other similar computing devices. The components shown herein, their connections and relationships, and their functions are merely illustrative and are not intended to limit the implementation of the present disclosure described and / or claimed herein.
[0179] Device 600 includes a computing unit 601, which can perform various appropriate actions and processes based on a computer program stored in read-only memory (ROM) 602 or a computer program loaded from storage unit 608 into random access memory (RAM) 603. The RAM 603 may also store various programs and data required for the operation of device 600. The computing unit 601, ROM 602, and RAM 603 are interconnected via bus 604. An input / output (I / O) interface 605 is also connected to bus 604.
[0180] Multiple components in device 600 are connected to I / O interface 605, including: input unit 606, such as keyboard, mouse, etc.; output unit 607, such as various types of monitors, speakers, etc.; storage unit 608, such as disk, optical disk, etc.; and communication unit 609, such as network card, modem, wireless transceiver, etc. Communication unit 609 allows device 600 to exchange information / data with other devices through computer networks such as the Internet and / or various telecommunications networks.
[0181] The computing unit 601 can be a variety of 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 special-purpose 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 performs the various methods and processes described above, such as method 100. For example, in some embodiments, method 100 may be implemented as a computer software program tangibly contained in a machine-readable medium, such as storage unit 608. In some embodiments, part or all of the computer program may be loaded and / or installed on device 600 via ROM 602 and / or communication unit 609. When the computer program is loaded into RAM 603 and executed by the computing unit 601, one or more steps of method 100 described above may be performed. Alternatively, in other embodiments, the computing unit 601 may be configured to perform method 100 by any other suitable means (e.g., by means of firmware).
[0182] Various embodiments of the systems and techniques described above herein can be implemented in digital electronic circuit systems, integrated circuit systems, field-programmable gate arrays (FPGAs), application-specific integrated circuits (ASICs), application-specific standard products (ASSPs), systems-on-a-chip (SoCs), payload-programmable logic devices (CPLDs), computer hardware, firmware, software, and / or combinations thereof. These various embodiments may include implementations in one or more computer programs that can be executed and / or interpreted on a programmable system including at least one programmable processor, which may be a dedicated or general-purpose programmable processor, capable of receiving data and instructions from a storage system, at least one input device, and at least one output device, and transmitting data and instructions to the storage system, the at least one input device, and the at least one output device.
[0183] The program code used to implement the methods of this disclosure may be written in any combination of one or more programming languages. This program code may be provided to a processor or controller of a general-purpose computer, special-purpose computer, or other programmable data processing apparatus, such that when executed by the processor or controller, the program code causes the functions / operations specified in the flowcharts and / or block diagrams to be implemented. The program code may be executed entirely on a machine, partially on a machine, as a standalone software package partially on a machine and partially on a remote machine, or entirely on a remote machine or server.
[0184] In the context of this disclosure, a machine-readable medium can be a tangible medium that may contain or store a program for use by or in conjunction 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 be, 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 machine-readable storage media include electrical connections based on one or more wires, portable computer disks, hard disks, random access memory (RAM), read-only memory (ROM), erasable programmable read-only memory (EPROM or flash memory), optical fiber, portable compact disk read-only memory (CD-ROM), optical storage devices, magnetic storage devices, or any suitable combination of the foregoing.
[0185] To provide interaction with a user, the systems and techniques described herein can be implemented on a computer having: a display device for displaying information to the user (e.g., a CRT (cathode ray tube) or LCD (liquid crystal display) monitor); and a keyboard and pointing device (e.g., a mouse or trackball) through which the user provides input to the computer. Other types of devices can also be used to provide 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 sound input, voice input, or tactile input).
[0186] The systems and technologies described herein can be implemented in computing systems that include backend components (e.g., as a data server), or computing systems that include middleware components (e.g., an application server), or computing systems that include frontend components (e.g., a user computer with a graphical user interface or web browser through which a user can interact with embodiments of the systems and technologies described herein), or any combination of such backend, middleware, or frontend components. The components of the system can be interconnected via digital data communication of any form or medium (e.g., a communication network). Examples of communication networks include local area networks (LANs), wide area networks (WANs), and the Internet.
[0187] Computing systems can include clients and servers. Clients and servers are generally located far apart and typically interact via communication networks. Client-server relationships are created by computer programs running on the respective computers and having a client-server relationship with each other. Servers can be cloud servers, servers in distributed systems, or servers incorporating blockchain technology.
[0188] It should be understood that the various forms of processes shown above can be used to reorder, add, or delete steps. For example, the steps described in this disclosure can be executed in parallel, sequentially, or in different orders, as long as the desired result of the technical solution disclosed in this disclosure can be achieved, and this is not limited herein.
[0189] The specific embodiments described above do not constitute a limitation on the scope of protection 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 should be included within the scope of protection of this disclosure.
Claims
1. A method for obtaining the thermal correction coefficient of an intermittent device, characterized in that, include: During the chemical reaction in the intermittent equipment, the fully automatic reaction calorimeter is controlled to operate in isothermal mode to measure the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops. The intermittent equipment is located inside the fully automatic reaction calorimeter and is the reaction vessel controlled by the fully automatic reaction calorimeter. In the isothermal mode, the fully automatic reaction calorimeter controls the temperature of the material in the intermittent equipment to remain constant. During the chemical reaction in the intermittent equipment, the fully automatic reaction calorimeter is controlled to operate in adiabatic mode to obtain the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops. In the adiabatic mode, the temperature of the jacket wrapped around the outer wall of the intermittent equipment is controlled by the fully automatic reaction calorimeter to change synchronously with the material temperature. The equipment parameters are related to the heat transfer coefficient and heat transfer area of the intermittent equipment. Based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment, the thermal correction coefficient of the intermittent equipment is obtained.
2. The method according to claim 1, characterized in that, The measured theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops includes: The exothermic enthalpy and specific heat capacity of the intermittent equipment are obtained by measuring the fully automated reaction calorimeter. Obtain the initial total mass of materials added to the intermittent equipment; The theoretical adiabatic temperature rise is calculated based on the exothermic enthalpy, the specific heat capacity, and the initial total mass of the material.
3. The method according to claim 1, characterized in that, The control of the fully automatic reaction calorimeter to operate in adiabatic mode includes: According to the preset temperature rise step, the material temperature in the intermittent equipment is gradually increased, and the jacket temperature corresponding to the material temperature is calculated simultaneously to synchronously control the jacket temperature.
4. The method according to claim 3, characterized in that, The calculation of the jacket temperature corresponding to the material temperature includes: Obtain a pre-stored adiabatic temperature relationship between the material temperature and the jacket temperature, wherein the adiabatic temperature relationship is determined based on at least one of the following: the type of the intermittent equipment, the type of material, and the temperature difference between the jacket temperature and the material temperature. Based on the material temperature inside the intermittent equipment and the adiabatic temperature relationship, the jacket temperature corresponding to the material temperature is calculated.
5. The method according to claim 1, characterized in that, The equipment parameters of the intermittent equipment are obtained through the following steps: After the chemical reaction stops, while keeping the material temperature constant, the heating device is controlled to perform a first heating operation on the material in the intermittent equipment, and the heating heat used in the first heating operation is obtained; The first temperature difference between the jacket and the material is obtained when the temperature of the jacket stops changing under the heating heat and the heat absorption of the jacket. The equipment parameters are calculated based on the heating heat and the first temperature difference.
6. The method according to claim 5, characterized in that, The specific heat capacity of the material is obtained through the following steps: After calculating the equipment parameters, the heating device is controlled to perform a second heating operation on the material in the intermittent equipment, and heating is stopped when the temperature rise of the material reaches the preset temperature rise. Under the second heating operation, obtain the second temperature difference between the jacket and the material, and the heating rate of the material in the intermittent device; The specific heat capacity of the material is calculated based on the equipment parameters, the second temperature difference, the mass of the material in the intermittent equipment, and the material heating rate.
7. The method according to any one of claims 1 to 6, characterized in that, The step of obtaining the thermal correction coefficient of the intermittent equipment based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment includes: Based on the preset heat balance formula for material reaction, a curve showing the relationship between thermal time parameters, reaction time, and temperature difference between the jacket and the material is obtained. The thermal time parameter is a function of the thermal correction coefficient, the total initial mass of material added to the intermittent equipment, the specific heat capacity of the material, and the equipment parameters. The thermal time parameter is obtained by processing the relationship curve. The thermal correction factor of the intermittent equipment is calculated based on the thermal time parameter, the theoretical adiabatic temperature rise, and the actual adiabatic temperature rise.
8. The method according to claim 7, characterized in that, The step of calculating the thermal correction factor for the intermittent equipment based on the thermal time parameter, the theoretical adiabatic temperature rise, and the actual adiabatic temperature rise includes: The theoretical thermal correction coefficient is calculated based on the thermal time parameter, the initial total mass of the material, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment. Calculate the actual thermal correction factor based on the theoretical adiabatic temperature rise and the actual adiabatic temperature rise; The theoretical thermal correction factor is verified based on the actual thermal correction factor. If the verification passes, the theoretical thermal correction factor is taken as the final thermal correction factor.
9. A device for obtaining the thermal correction coefficient of an intermittent device, characterized in that, include: The first processing module is used to control the fully automatic reaction calorimeter to operate in isothermal mode during the chemical reaction in the intermittent equipment, so as to measure the theoretical adiabatic temperature rise of the material in the intermittent equipment when the chemical reaction stops. The intermittent equipment is located inside the fully automatic reaction calorimeter and is the reaction vessel to be controlled by the fully automatic reaction calorimeter. In the isothermal mode, the fully automatic reaction calorimeter controls the temperature of the material in the intermittent equipment to remain constant. The second processing module is used to control the fully automatic reaction calorimeter to operate in adiabatic mode during the chemical reaction in the intermittent equipment, and to obtain the actual adiabatic temperature rise of the material in the intermittent equipment, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment when the chemical reaction stops. In the adiabatic mode, the fully automatic reaction calorimeter controls the temperature of the jacket wrapped around the outer wall of the intermittent equipment to change synchronously with the material temperature. The equipment parameters are related to the heat transfer coefficient and heat transfer area of the intermittent equipment. The acquisition module is used to acquire the thermal correction coefficient of the intermittent equipment based on the theoretical adiabatic temperature rise, the actual adiabatic temperature rise, the specific heat capacity of the material, and the equipment parameters of the intermittent equipment.
10. An electronic device, characterized in that, include: At least one processor; as well as A memory communicatively connected to the at least one processor; wherein, The memory stores instructions that can be executed by the at least one processor to enable the at least one processor to perform the method of any one of claims 1-8.
Citation Information
Patent Citations
Method, device and equipment for acquiring thermal correction coefficient of intermittent equipment
CN117030789A