An adiabatic accelerating calorimetry method with fast reaction heat loss correction

Abstract

The application discloses an adiabatic accelerating calorimetry method with fast reaction heat loss correction. The application realizes more accurate calculation of sample reaction kinetics and thermodynamics by compensating the convection and conduction heat loss in the fast reaction stage; differential equations are derived and solved from the perspective of heat balance by using heat transfer analysis; a new heat loss calibration mode is added, the HWS heating stage is divided into two parts, the convection heat loss coefficient is calibrated by tracking the reaction system temperature by controlling the cover temperature in the first part, and the conduction heat loss coefficient is calibrated by controlling the constant temperature of the furnace body in the second part; the linear fitting and interpolation method are used to solve the relationship between the heat loss coefficient and the temperature in the reaction process; and finally, the heat loss in the reaction process is integrated to compensate the sample heat release. The application improves the accuracy and reliability of the solution of thermodynamic and kinetic parameters.

Description

Technical Field

[0001] This invention relates to the field of accelerated calorimetry technology for chemical process safety, and specifically to an adiabatic accelerated calorimetry method with rapid reaction heat loss correction. Background Technology

[0002] The adiabatic accelerated calorimeter (ARC) was first developed by Dow Chemical Company in the United States. [1] Accelerated calorimeters are used for thermal stability hazard assessment. Typically, they operate in a heating-wait-search (HWS) mode. [2] The process involves first heating the sample to a preset temperature, then waiting for a period of time to allow the sample and the adiabatic furnace to reach thermal equilibrium. Next, it detects whether the sample releases heat. If no heat is released, the sample is heated to the next temperature point to begin a new cycle of "heating-waiting-searching." During the search phase, the sample reaction is detected by real-time assessment of the temperature rise rate, which must exceed a set detection threshold. If the rate exceeds the threshold, a reaction is detected, and the process then enters the tracking phase. Thermodynamic and thermodynamic analyses are performed on the temperature-time series data from this tracking phase to predict the thermal hazard of the chemical substance. Adiabatic accelerated calorimeters are widely used in research fields such as chemical process optimization and scale-up, chemical thermal hazard assessment, and thermal stability evaluation.

[0003] Existing adiabatic accelerated reaction calorimeters typically use metal sample cells capable of withstanding high temperatures and pressures to hold the samples. However, in actual testing, the sample cell and sample must be considered as a single unit (hereinafter referred to as the reaction system), and this system is considered adiabatic to the environment during the tracking phase. Because the sample cell has a certain mass and heat capacity, when an exothermic reaction occurs during the test, some of the released heat will be absorbed by the sample cell, resulting in exothermic heat loss. Researchers in related fields have proposed a correction theory for the thermal inertia factor. [3] This is the ratio of the thermal effect of the reaction system (including the sample and sample container) to the thermal effect of the sample. The thermal inertia factor is used to correct the adiabatic data in an attempt to eliminate errors generated in the study of thermal analysis kinetics.

[0004] However, when performing thermal analysis on some high-concentration, rapidly exothermic chemical reactions, even after correcting for thermal inertia factors, the results of adiabatic accelerated calorimetry (ARC) experiments still exhibit significant errors. This is mainly due to issues such as the dynamic heating response of the ARC furnace and heat loss within the mechanical components, resulting in the sample reaction occurring under non-adiabatic conditions and exhibiting a "thermal hysteresis" phenomenon in the furnace temperature during the intense reaction phase of adiabatic tracking. Simply considering thermal inertia factors cannot completely correct for the heat loss in the reaction system. Related experimental analyses show that when high-concentration samples react, the reaction system cannot remain in an adiabatic state indefinitely; convective heat transfer occurs between the reaction system and the ARC furnace body, as well as conductive heat transfer with the furnace lid.[4] Although the patent "An Adiabatic Accelerated Calorimeter with Dynamic Thermal Inertia Correction Features" (Patent No.: CN109974902B) recognized this problem and invented an adiabatic accelerated calorimeter device for correcting dynamic thermal inertia factors. [5] This ensures the adiabatic tracking performance of ARC during sample reaction, but its sample cell adopts a dual-channel design, which is complex and has poor feasibility in actual experiments, making it inconvenient to upgrade and modify existing ARC instruments commonly used in the market.

[0005] In current industry research, it is generally assumed that the reaction system is in an adiabatic experimental environment throughout the entire thermal analysis experiment. It is considered that the convective heat loss between the reaction system and the ARC furnace body has no impact on the total heat released by the reaction. At the same time, the conductive heat loss caused by the fit between the metal sample cell and the connecting parts is ignored. Research on this part of conductive heat loss is relatively limited in the industry, and it can be said that there is a lack of systematic research on solutions to this problem. As an important analytical instrument for the causes of thermal safety accidents, the adiabatic accelerated calorimeter, due to its limited adiabatic performance, can cause errors in the calculation of parameters characterizing thermal hazards, such as adiabatic temperature rise and thermal decomposition kinetics, in the assessment of hazardous chemicals. This can affect the assessment of the hazard level of chemical processes and potentially lead to serious consequences. This invention, starting from the perspective of heat loss caused by the adiabatic accelerated calorimeter device itself, conducts theoretical and experimental analysis and proposes a method for correcting heat loss during the adiabatic tracking process of the adiabatic accelerated calorimeter.

[0006] References

[0007] [1] Townsend, DI; Solem, RH; Timm, EE; Caldecourt, VJAcceleratingRate Calorimeter and Method of Operation [P]. US 4, 208, 907, 1980.

[0008] [2] Wang Jichen. Research on evaluation and improvement methods of adiabatic performance of accelerated calorimeter [D]. China Jiliang University, 2019.

[0009] [3]Townsend DI,Tou J C.Thermal hazard evaluation by an acceleratingrate calorimeter[J].Thermochimica Acta,1980,37(1):1-30.

[0010] [4]Min Sheng; Daniel Valco; Craig Tucker; Heat Loss in Accelerating RateCalorimetry Analysis and Thermal Lag for High Self-Heat Rates.Org.ProcessRes.2021 25(1),108-119.

[0011] [5] Ye Shuliang, Ding Jiong, Wang Jichen. An adiabatic accelerating calorimeter with dynamic thermal inertia correction characteristics [P]. Zhejiang Province: CN109974902B, 2020-09-11. Summary of the Invention

[0012] To address the shortcomings of existing technologies, this invention combines heat transfer theory and thermal balance to propose an adiabatic accelerated calorimetry method with rapid response and heat loss correction.

[0013] This invention includes the following steps:

[0014] Step 1: Analyze the heat generation inside the adiabatic accelerated calorimeter during the adiabatic tracking stage using heat transfer analysis, and create a heat conduction differential equation based on the principle of heat balance.

[0015] Step 2: Using the obtained reaction system and furnace temperature, solve for the convective heat loss coefficient and the conductive heat loss coefficient of the reaction system, and correct for heat loss.

[0016] Step 3: Correct the heat of reaction of the sample based on the heat loss of each part, and further correct the sample temperature rise rate.

[0017] In step 2, the entire experimental process is divided into three parts: before the reaction, during the reaction, and after the reaction.

[0018] At any step before or after the reaction, the heating phase can be divided into two parts:

[0019] First half: When the furnace body heating time reaches half of the heating stage time, the furnace wall and furnace bottom are kept at a constant temperature, the furnace cover tracks the temperature of the reaction system, the temperature of the furnace cover is the same as that of the reaction system, and the convective heat dissipation loss coefficient of the reaction system and the furnace body is calibrated.

[0020] The latter half: The furnace cover, furnace wall, and furnace bottom are kept at a constant temperature. Convection and conduction heat loss occur simultaneously. The sum of the coefficients for convection and conduction heat loss terms is calibrated.

[0021] By fitting the reaction system and furnace temperature to the time function, a series of relationships between the convective heat dissipation loss coefficient and the step temperature before and after the reaction, as well as the conductive heat dissipation loss coefficient and the step temperature, were obtained.

[0022] Using the Lagrange interpolation method, the relationship between the convective heat dissipation loss coefficient and the conduction heat dissipation loss coefficient in the reaction and temperature is derived;

[0023] By using integral calculations to measure heat loss through conduction and convection, the heat of reaction during the reaction can be corrected.

[0024] The present invention also provides an application of the above method in an exothermic reaction experiment of a high concentration of chemical substances.

[0025] The beneficial effects of this invention are as follows: For the thermal hysteresis phenomenon that occurs in the exothermic reaction process of high-concentration chemical substances, this invention proposes a calculation method for the conductive heat loss between the metal sample cell and the joint components, as well as the convective heat loss between the metal sample cell and the furnace body, by adding a new calibration mode and utilizing differential, fitting, and interpolation analysis methods. This effectively corrects the sample's temperature rise rate. Compared with traditional adiabatic accelerated calorimetry methods, it can more accurately reflect the thermal decomposition process of the sample, thereby solving for more accurate sample thermal decomposition reaction kinetics and thermodynamic parameters. Attached Figure Description

[0026] Figure 1 This is a diagram of the HWS heat dissipation calibration mode in this invention;

[0027] Figure 2 Diagram of the mechanical device for the accelerated calorimeter;

[0028] Figure 3 This is a diagram showing the assembly of the metal sample cell and the furnace lid.

[0029] Figure 4 This is a flowchart of a temperature control algorithm for an adiabatic accelerated calorimetry method with rapid response heat loss correction. Detailed Implementation

[0030] The design concept of this invention is described as follows: Based on the traditional HWS mode, a new temperature control mode (HWS heat loss calibration mode) is proposed. Figure 1As shown, the heating stage is divided into two phases. In the first phase, the furnace wall and bottom are rapidly kept at a constant temperature to the target step temperature, while the furnace lid tracks the temperature of the reaction system. In the second phase, the furnace wall, bottom, and lid are rapidly kept at a constant temperature to the step temperature. This temperature control mode is used to obtain the temperature change of the reaction system, and the convective and conductive heat dissipation coefficients at the step temperatures are calculated. The furnace body temperature and reaction system temperature before and after the reaction are fitted to a time function to obtain the convective and conductive heat dissipation coefficients for each step temperature. Then, using the convective and conductive heat dissipation coefficients for each step temperature, Lagrange interpolation is used to derive the convective and conductive heat dissipation coefficients during the adiabatic reaction process. Finally, integration is used to calculate the convective and conductive heat dissipation terms during the reaction. This invention can improve the thermal hysteresis phenomenon in the violently exothermic phase of high-concentration chemical reaction processes, correct the heat loss in the adiabatic tracking phase, and improve the accuracy and reliability of solving thermodynamic and kinetic parameters.

[0031] Based on the above concept, this invention utilizes heat transfer analysis of the internal heat generation of an adiabatic accelerated calorimeter during the adiabatic tracking stage, and combines this with the principle of heat balance to create a heat conduction differential equation. The obtained reaction system and furnace temperature are used to solve for the convective and conductive heat loss terms of the reaction system, correcting for heat loss. The heat of reaction of the sample is corrected based on the heat loss of each component, and the sample temperature rise rate is further corrected, thereby improving the accuracy of the calculations of chemical kinetics and thermodynamics.

[0032] The technical principle of this invention is as follows:

[0033] In adiabatic accelerated calorimeter, under thermal equilibrium conditions, the amount of heat Q generated by the system is... 吸收 =Q 总 -Q 损失 The principle, in which Q 吸收 Including part of the heat absorbed by the reaction system; Q 损失 This includes convective heat loss between the reaction system and the ARC furnace body, and conductive heat loss between the reaction system and the joint components.

[0034] Using the knowledge of heat transfer, we conduct a theoretical analysis of the adiabatic tracking stage of the sample reaction and list the following heat conduction differential equation:

[0035]

[0036] The two terms on the left side of equation (1) represent the heat absorbed by the sample and the heat absorbed by the metal sample cell, respectively. s For sample quality, c s The specific heat capacity of the sample; m b For the mass of the metal sample cell, c b dT / dt represents the specific heat capacity of the metal sample cell; dT / dt represents the temperature rise rate of the sample.

[0037] ms ΔH r dα / dt is the total heat production term of the sample during the reaction process, ΔH r The heat released per unit mass is α, and the sample conversion rate is α.

[0038] hA(T-T0) represents the convective heat loss between the reaction system and the ARC furnace. h is the convective heat transfer coefficient, A is the convective heat transfer area, T is the temperature of the reaction system measured by the thermocouple of the metal sample cell, and T0 is the temperature of the furnace wall measured by the thermocouple.

[0039] k f A f (TT f ) / δ f This represents the heat dissipation term through conduction between the reaction system and the connecting components. f δ represents the thermal conductivity between the reaction system and the furnace cover. f For the thermal conduction gradient between the reaction system and the furnace cover, A f T represents the heat transfer contact area between the furnace cover and the reaction system. f The temperature value was measured by the thermocouple on the furnace cover.

[0040] The convective heat loss and conductive heat loss terms on the right side of equation (1) can be calibrated using the HWS heat loss calibration experiment. Where T, T0, and T... f The convective heat dissipation coefficient hA and the conductive heat dissipation coefficient k can be further calculated using a calorimeter. f A f / δ f The specific values ​​are used to correct the sample temperature rise rate, achieving the purpose of thermodynamic correction and improving the accuracy of reaction kinetics and thermodynamic solutions.

[0041] The heat dissipation term in equation (1) can be calibrated by the HWS interpolation calibration experiment, the principle of which is as follows:

[0042] To correct for heat loss during the exothermic reaction of high-concentration samples, this invention employs the HWS heat loss calibration experiment (described in detail below) to correct for heat loss during the sample's exothermic process.

[0043] The HWS heat dissipation calibration experiment employs a novel temperature control algorithm based on the classic HWS model. The entire experimental process is divided into three parts: before, during, and after the reaction. At any step before or after the reaction, the heating stage is divided into two parts. In the first half, the furnace body heating time reaches half of the heating stage time, the furnace bottom is kept at a constant temperature, and the furnace lid tracks the reaction system temperature. Since the furnace lid and reaction system temperatures are the same, the convective heat dissipation coefficients of the reaction system and the furnace body can be calibrated. In the second half, the furnace lid, furnace wall, and furnace bottom are kept at constant temperatures, and both convective and conductive heat dissipation occur simultaneously. At this point, the sum of the convective and conductive heat dissipation coefficients can be calibrated. After the reaction, the HWS step is run again using the same temperature control method. By fitting the reaction system and furnace body temperatures to time, a series of relationships between the convective and conductive heat dissipation coefficients before and after the reaction and the step temperature can be obtained. Then, using Lagrange interpolation, the relationship between the convective and conductive heat dissipation coefficients and temperature during the reaction is derived. Then, the heat loss due to conduction and convection is calculated by integral calculation to correct the heat of reaction during the reaction. Finally, the kinetic parameters of thermal analysis are solved by nonlinear fitting of the model.

[0044] In some embodiments, the specific steps of an adiabatic accelerated calorimetry method with rapid response heat loss correction are as follows:

[0045] a) Before the start of the adiabatic reaction experiment, measure the specific heat capacity c of the reaction tank. b With mass m b Determine the mass m of the sample s ;

[0046] b) During the experiment, the sample temperature was first raised to 20K before the initial reaction temperature. Temperature control was performed using the HWS heat dissipation calibration mode. The passive heating phase of the reaction system differed from the classic HWS mode; during the initial heating phase, the furnace bottom and furnace wall maintained a constant temperature, while the furnace wall tracked the sample cell temperature. When half of the target step heating time was reached, the furnace lid, furnace wall, and furnace bottom maintained a constant temperature.

[0047] c) The time when the HWS starting step furnace wall and furnace bottom temperatures reach the target step temperature is defined as t1(0). The time when the heating time reaches half of the target temperature heating stage is defined as t2(0). The time when the waiting mode is entered is defined as t3(0). The temperature of the reaction system is collected every Δt. The temperature of the furnace body and sample cell is recorded from t1(0) to t2(0), and the temperature of the sample and furnace body / furnace lid is recorded from t2(0) to t3. The n steps before the reaction are recorded according to the specific reaction settings.

[0048] d) After the tracking is completed, continue executing the HWS heat dissipation calibration mode step to obtain the temperature of the reaction system. Similarly, the time when the initial step furnace wall and furnace bottom temperatures after the sample reaction reach the target furnace step temperature is recorded as t1(n). The time when the heating time reaches half of the target step heating time after the reaction is completed is recorded as t2(n). The time when the heating stage ends and the waiting stage begins is recorded as t3(n). The temperature of the reaction system is collected every Δt time interval. The temperatures of the furnace body and sample cell are recorded from time t1(n) to time t2(n), and the temperatures of the sample and furnace body / furnace lid are recorded from time t2(n) to time t3(n). Record n ​​steps after the reaction according to the specific reaction settings.

[0049] e) After the reaction is complete, the temperature-time signal of the sample process is obtained. The differential calculation is performed on this signal to obtain the temperature rise rate-time signal of the sample.

[0050] f) By fitting the furnace wall temperature and the temperature and time of the reaction system from t1(m) to t2(m) (m is 0, 1, 2...n-1), the relationship between the convective heat dissipation coefficient before the reaction and the step temperature can be derived. By fitting the temperature of the reaction system and the furnace wall and furnace cover as a function of time from t2(m) to t3(m), the relationship between the coefficients of the convective and conductive heat dissipation terms before the reaction and the step temperature can be derived. Thus, the relationship between the convective heat dissipation coefficient and the conductive heat dissipation coefficient before the reaction and the step temperature can be obtained. Similarly, from the step temperature after the reaction, the relationship between the convective heat dissipation coefficient and the conductive heat dissipation coefficient after the reaction and the step temperature can be derived.

[0051] g) Using the relationship between the convective and conductive heat dissipation coefficients and the step temperature obtained in step f, derive the relationship between the convective and conductive heat dissipation coefficients and temperature during the reaction using Lagrange interpolation. Then, use integral calculations to obtain the heat loss during the reaction and correct for the heat loss during the reaction process. Finally, use model fitting to solve for the kinetic parameters.

[0052] Based on the above embodiments, combined with Figure 4 Using classical accelerating calorimeters (such as...) Figure 2 As shown), the assembly diagram of its furnace cover sample pool (as shown) Figure 3 As shown in the figure, it includes a furnace cover 1, a weld resist connector 2, an internal hex nut 3, a compression fitting 4, and a sample cell 5. The experimental procedure is as follows:

[0053] Turn on the ARC instrument, set the start and end temperature points. The temperature range can be adjusted according to the specific sample reaction temperature range. Set it to 20℃ before the sample reference reaction starts, with a temperature increment of 5℃. The temperature step time for each temperature step is 30min. After the reaction ends, the temperature increment is 5℃, and the number of steps after the reaction ends is 4. Start the HWS heat dissipation calibration experiment. During the heating stage, the furnace bottom and furnace wall are heated to the target step temperature and then kept at a constant temperature. The furnace lid tracks the sample cell temperature within Δt1 time to correct the conduction heat dissipation term in formula (1), simplifying the heat balance formula to:

[0054]

[0055] Given the boundary conditions under the HWS mode, i.e., the initial temperature of the reaction system is the temperature of the previous step, and the final temperature is the target step temperature, solving equation (2) yields the following:

[0056]

[0057] Where ΔT is the step size of the temperature rise, taking the logarithm of formula (3) yields formula (4). From formula (4), the temperature of the reaction system and the furnace wall temperature are related to time within the heating stage Δt2 before and after the reaction. Using linear fitting, the hA of each temperature step is obtained. i (i is 0-7).

[0058]

[0059] When the reaction system and furnace body enter the heating stage Δt2, the furnace cover temperature T is at this time. f When the furnace wall temperature is equal to T0, formula (1) can be simplified to:

[0060]

[0061] Similarly, by solving a series of temperature difference data Δt2 during the heating stages before and after the reaction, as well as the differential equation of temperature versus time in the reaction system, formula (6) is obtained:

[0062]

[0063] hA for each step obtained from formula (4) i And each step (hA+k) obtained by linear fitting method of formula (6) f A f / δ f ) i The solution can be obtained as (k) f A f / δ f ) iThen, using formulas (7) and (8), the relationship between the convective heat loss coefficient hA of the reaction system and the furnace wall and the temperature is calculated by Lagrange interpolation.

[0064]

[0065]

[0066] The same method can be used to obtain the heat dissipation coefficient j. f A f / δ f Regarding the relationship with temperature, considering that the heat dissipation coefficients of convection and conduction are related to temperature, formula (9) can be obtained from formula (1):

[0067]

[0068] Integrate equation (9) and interpolate the resulting hA(T) with (k f A f / δ f Substituting (T) into the equation, the heat of reaction and heat loss can be calculated:

[0069]

[0070] T onset T is the time at which the reaction begins. final At the end of the reaction, α onset α represents the conversion rate of the sample at the start of the reaction (typically taken as 0). final This represents the conversion rate of the sample at the end of the reaction, which is typically 1 when the reaction is complete. The conversion rate α during the reaction is related to ΔH. r The correspondence between T is as follows:

[0071]

[0072] For elementary reactions, namely:

[0073]

[0074] Where r is the chemical reaction rate of the reaction system, dα / dt is the rate of change of reaction conversion, k(T) is the temperature relationship of the rate constant, E is the activation energy of the reaction, k0 is the pre-exponential factor, R is the universal gas constant, α is calculated by formula (11), and n is the reaction order.

[0075] Substituting equation (11) into equation (12) will establish a self-reaction exothermic equation, yielding the reaction model:

[0076]

[0077] Where dT修正 / dt is the corrected temperature rise rate, as shown in equation (14). Finally, by nonlinear fitting of the model in equation (13), the calculation of the three factors of thermal analysis kinetics (activation energy, pre-exponential factor, and reaction order) can be realized.

[0078]

[0079] In summary, this embodiment can be summarized as follows:

[0080] 1. The temperatures of the sample and the furnace cover, wall, and bottom of the furnace body were recorded by a calorimeter during all heating stages before and after the reaction. The temperature difference of the furnace wall sample pool during all heating stages was calculated in relation to time.

[0081] 2. Differentiate the temperature-time signal of the reaction system during the heating stage Δt1 to obtain the relationship between the sample temperature rise rate and time. Then, obtain the relationship between hA and the step temperature using formula (4).

[0082] 3. Differentiate the temperature-time signal of the reaction system during the heating stage Δt2 to obtain the relationship between the sample temperature rise rate and time. From formula (6), we can obtain hA+k f A f / δ f The relationship with the step temperature. From step 2, we can obtain k. f A f / δ f Relationship with step temperature.

[0083] 4. Solve for hA and k during the reaction using Lagrange interpolation. f A f / δ f Relationship with temperature.

[0084] 5. Solve for the convective and conductive heat loss during the reaction process by integrating.

[0085] The convective and conductive heat dissipation coefficients were obtained through the above implementation process, and the convective and conductive heat loss during the reaction was calculated, thus realizing the correction of formula (1). Based on this, this embodiment makes up for the gap in the calculation of convective and conductive heat loss by the adiabatic acceleration method, overcomes the shortcomings of the structure of the classic adiabatic acceleration calorimeter, and obtains more accurate thermodynamic parameters after reaction compensation heat loss.

Claims

1. An adiabatic accelerated calorimetry method with rapid response and heat loss correction, characterized in that: Step 1: Analyze the heat generation inside the adiabatic accelerated calorimeter during the adiabatic tracking stage using heat transfer analysis. Based on the principle of heat balance, create a heat conduction differential equation, which is expressed as follows: Where m s For sample quality, c s For the specific heat capacity of the sample, m b For the mass of the metal sample cell, c b dT / dt is the specific heat capacity of the metal sample cell, ΔH is the temperature rise rate of the sample, and dH is the temperature rise rate of the sample. r The heat released per unit mass is given by: α, sample conversion rate; h, convective heat transfer coefficient; A, convective heat transfer area; T, temperature measured by the thermocouple in the metal sample cell as the reaction system temperature; T0, temperature measured by the thermocouple on the furnace wall; k. f The thermal conductivity between the reaction system and the furnace cover. For the thermal conduction gradient between the reaction system and the furnace cover, A f T represents the heat transfer contact area between the furnace cover and the reaction system. f The temperature value was measured by the thermocouple on the furnace cover. Step 2: Using the obtained reaction system and furnace temperature, solve for the convective heat loss coefficient and the conductive heat loss coefficient of the reaction system, and correct for heat loss. Step 3: Correct the heat of reaction of the sample based on the heat loss of each part, and further correct the sample temperature rise rate; In step 2, the entire experimental process is divided into three parts: before the reaction, during the reaction, and after the reaction. At any step before or after the reaction, the heating phase can be divided into two parts: First half: When the furnace body heating time reaches half of the heating stage time, the furnace wall and furnace bottom are kept at a constant temperature, the furnace cover tracks the temperature of the reaction system, the temperature of the furnace cover is the same as that of the reaction system, and the convective heat dissipation loss coefficient of the reaction system and the furnace body is calibrated. The latter half: The furnace cover, furnace wall, and furnace bottom are kept at a constant temperature. Convection and conduction heat loss occur simultaneously. The sum of the coefficients for convection and conduction heat loss terms is calibrated. By fitting the reaction system and furnace temperature to the time function, a series of relationships between the convective heat dissipation loss coefficient and the step temperature before and after the reaction, as well as the conductive heat dissipation loss coefficient and the step temperature, were obtained. Using the Lagrange interpolation method, the relationship between the convective heat dissipation loss coefficient and the conduction heat dissipation loss coefficient in the reaction and temperature is derived; By using integral calculations to determine the conduction and convection heat loss, the heat of reaction during the reaction can be corrected. After the heat loss correction is completed, the kinetic parameters are solved by fitting a reaction model, which is expressed as follows: Where dT 修正 / dt is the corrected temperature rise rate. Pre-exponential factor, The activation energy of the reaction. It is a universal gas constant. denoted as the reaction order.

2. The adiabatic accelerated calorimetry method with rapid response heat loss correction according to claim 1, characterized in that: The convective heat dissipation loss factor is hA, and the conductive heat dissipation loss factor is... / .

3. The application of the adiabatic accelerated calorimetry method with rapid reaction heat loss correction as described in claim 1 or 2 in experiments on exothermic reactions of high-concentration chemical substances.

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