A continuous pipeline reaction heat testing method and system

Abstract

The present invention relates to the technical field of reaction heat detection, and particularly relates to a continuous pipeline reaction heat testing method and system, which comprises the following steps: obtaining reaction data, wherein the reaction data includes a reaction equation, the dosage of reactants, and the optimal reaction temperature Ty; putting a preset dosage of reactants into the continuous pipeline and performing a first temperature measurement; triggering reaction conditions to carry out the reaction; calculating the reaction heat Qf according to a formula. While ensuring the optimal reaction temperature, the present invention also transfers the heat generated by the reaction to a water tank through a heat exchange method, thereby making it more convenient to calculate the heat released during the reaction process.

Description

Technical Field

[0001] The present invention relates to the technical field of reaction heat detection, and particularly relates to a continuous pipeline reaction heat testing method and system. Background Art

[0002] Continuous pipeline reaction heat testing is an experimental method used to evaluate the thermal behavior of chemical reactions under continuous flow conditions. This method is usually used to study the heat release rate characteristics, safety performance, and thermal stability of chemical reactions, etc. In the specific testing process, a continuous flow pipeline reaction device needs to be set up in the laboratory first. This device includes a feeding system, a pipeline reaction device, a heating or cooling system, and a data acquisition system. The raw materials required for the reaction are gradually fed into the reaction pipeline according to the ratio through the feeding system, and the data acquisition system records the temperature change data provided by the sensors, so as to calculate the reaction heat released during the reaction process.

[0003] In the prior art, for the reaction heat testing method of continuous pipelines, it is mostly to adjust the continuous pipeline into an intermittent or semi-intermittent batch reaction, and then select the corresponding calorimeter to test the temperature change during the reaction process, and calculate the heat released or absorbed by the reaction according to the heat capacity and temperature change. The common reaction heat calculation formula is: Q = cmΔt, where c represents specific heat capacity, m represents mass, and Δt represents temperature change.

[0004] Although the above method can measure the corresponding reaction heat, it indirectly measures the temperature change in the reaction system. Therefore, in order to accurately measure the temperature change brought by the reaction heat, it is necessary to ensure that the reaction test device is as consistent as possible with the actual reaction device; therefore, in some relatively dangerous and special situations, adjusting the continuous pipeline into an intermittent or semi-intermittent batch reaction will lead to a decrease in reaction conversion rate, more intense reaction, and the reaction is prone to get out of control. In this case, it is very dangerous to measure by conventional methods. Summary of the Invention

[0005] The purpose of the present invention is to provide a continuous pipeline reaction heat testing method and system to solve the above technical problems.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] A continuous pipeline reaction heat testing method includes a continuous pipeline used as a reaction vessel and a cooling jacket arranged on the continuous pipeline, and a plurality of temperature sensors are arranged on the continuous pipeline, and a heat exchange water tank is also arranged on the cooling jacket, and includes the following steps:

[0008] Obtain reaction data, where the reaction data includes a reaction equation, reactant dosage, and the optimal reaction temperature Ty;

[0009] Inject a preset dose of reactants into the continuous pipeline, and conduct the first temperature measurement. Collect the real-time data of each temperature sensor and take the average value as the initial reaction temperature T0.

[0010] Trigger the reaction conditions to conduct the reaction, and monitor the real-time temperature Ts of the reactants inside the continuous pipeline in real time. When the real-time temperature Ts = Ty, start the cooling jacket to cool down, so as to keep the real-time temperature of the reactants inside the continuous pipeline within the temperature range (Ty - 1.75K, Ty + K), where K is the preset temperature margin.

[0011] When, as the reaction proceeds, the real-time temperature Ts ≤ Ty - 1.75K, continue to cool the continuous pipeline through the cooling jacket. When the real-time temperature Ts = T0, partially close the cooling jacket. The partial closing means stopping the heat exchange between the cooling jacket and the continuous pipeline, and still retaining the heat exchange between the cooling jacket and the heat exchange water tank until the cooling medium in the cooling jacket returns to the initial heat exchange temperature and then completely closes.

[0012] Calculate the reaction heat Qf according to the formula. The specific formula is: Qf = cmΔt, where c represents the specific heat capacity of the cooling water, m represents the mass of the cooling water in the cooling water tank, and Δt represents the temperature rise of the cooling water in the cooling water tank.

[0013] As a further solution of the present invention: The specific steps for calculating the real-time temperature Ts are as follows:

[0014] A static mixer is preset inside the pipeline to ensure uniform mixing of the reactants inside the continuous pipeline.

[0015] Obtain the real-time measurement data of several temperature sensors. When the difference between any two real-time measurement data is less than or equal to the preset measurement error, take the average value of the several real-time measurement data as the real-time temperature Ts of the reactants inside the continuous pipeline. At the same time, the heat release rate at different positions of the pipeline can be measured and calculated in real time.

[0016] As a further solution of the present invention: When the difference between any two real-time measurement data among the real-time measurement data of several temperature sensors is greater than the preset measurement error, re-obtain the real-time measurement data of the temperature sensors.

[0017] As a further solution of the present invention: It further includes a standby water tank. After the cooling jacket is partially closed, when the temperature of the cooling medium in the cooling jacket is greater than the initial heat exchange temperature and less than or equal to (T' + t), close the heat exchange between the cooling jacket and the heat exchange water tank, and conduct the heat exchange between the cooling jacket and the standby water tank, where T' represents the temperature of the cooling water in the cold water tank, and t represents the preset heat exchange temperature difference.

[0018] As a further solution of the present invention: a standby water tank is connected to the cooling jacket. After the cooling medium in the cooling jacket returns to the initial heat exchange temperature, the calculation formula for the reaction heat is: Qf = c(mΔt + m'Δt'), where m' represents the mass of the cooling water in the standby water tank, and Δt represents the temperature rise of the cooling water in the standby water tank.

[0019] As a further solution of the present invention: the cooling jacket is provided with multiple circuits, including a reaction heat exchange circuit, a cooling circuit, a standby heat exchange circuit, and a standby cooling circuit. In the reaction heat exchange circuit, the cooling jacket exchanges heat between the continuous pipeline and the cooling water tank at the same time; in the cooling circuit, the cooling jacket exchanges heat only with the cooling water tank; in the standby heat exchange circuit, the cooling jacket exchanges heat between the continuous pipeline and the standby water tank at the same time; in the standby cooling circuit, the cooling jacket exchanges heat only with the standby water tank.

[0020] As a further solution of the present invention: when the temperature difference between the cooling water in the cooling water tank and the continuous pipeline is less than a preset value, switch the heat exchange circuit to the standby heat exchange circuit, and after partially closing the cooling jacket, perform heat exchange through the standby cooling circuit.

[0021] A continuous pipeline reaction heat test system includes a continuous pipeline used as a reaction vessel and a cooling jacket provided on the continuous pipeline. A plurality of temperature sensors are provided on the continuous pipeline, and a heat exchange water tank is also provided on the cooling jacket, including:

[0022] Initialization module: obtain reaction data, where the reaction data includes a reaction equation, reactant dosage, and the optimal reaction temperature Ty;

[0023] Pretreatment module: put a preset dosage of reactants into the continuous pipeline, perform the first temperature measurement, collect the real-time data of each temperature sensor, and take the average value as the initial reaction temperature T0;

[0024] Reaction control module: trigger reaction conditions, perform the reaction, and monitor the real-time temperature Ts of the reactants inside the continuous pipeline in real time. When the real-time temperature Ts = Ty, start the cooling jacket to cool down, so as to keep the real-time temperature of the reactants inside the continuous pipeline within the temperature range (Ty - 1.75K, Ty + K), where K is a preset temperature margin;

[0025] Reaction heat calculation module: When, as the reaction proceeds, the real-time temperature Ts ≤ Ty - 1.75K, the continuous pipeline is further cooled through the cooling jacket. When the real-time temperature Ts = T0, the cooling jacket is partially closed. The partial closure means stopping the heat exchange between the cooling jacket and the continuous pipeline, while still retaining the heat exchange between the cooling jacket and the water tank for heat exchange. It is completely closed until the cooling medium in the cooling jacket returns to the initial heat exchange temperature.

[0026] Calculate the reaction heat Qf according to the formula. The specific formula is: Qf = cmΔt, where c represents the specific heat capacity of the cooling water, m represents the mass of the cooling water in the cooling water tank, and Δt represents the temperature rise of the cooling water in the cooling water tank.

[0027] Advantages of the present invention: In the solution of the present invention, the reaction process is placed in a continuous pipeline, and the inside of the pipeline is in continuous flow, that is, a common loop-shaped or circular pipeline, and the material is circulated through end-to-end connection. Therefore, the present invention is mainly directed to the reaction heat test method for a solution reaction system, and has poor effects on reaction systems that do not have fluidity or have poor fluidity or whose products will precipitate and condense.

[0028] In the present invention, through an externally provided cooling jacket, the temperature change of the continuous pipeline during the reaction process can be controlled, so that the reaction rate can be controlled, which is safer, and the generation of side reactions or by-products can be effectively avoided. And because corresponding material changes will also occur during the reaction process, such as the generation of gas, etc., the continuous pipeline in the present invention can effectively increase the reaction safety. Secondly, while ensuring the optimal reaction temperature in the present invention, the heat generated by the reaction is transferred to the water tank through heat exchange, making it more convenient to calculate the heat released during the reaction process. Description of the Drawings

[0029] The present invention will be further described below with reference to the accompanying drawings.

[0030] Figure 1 It is a flow schematic diagram of a method for testing the reaction heat of a continuous pipeline in the present invention. Detailed Embodiments

[0031] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0032] Please refer to Figure 1As shown in the figure, the present invention is a method for testing the reaction heat of a continuous pipeline, including a continuous pipeline used as a reaction vessel and a cooling jacket provided on the continuous pipeline, and a plurality of temperature sensors are provided on the continuous pipeline, and a heat exchange water tank is also provided on the cooling jacket, including the following steps:

[0033] Obtain reaction data, where the reaction data includes a reaction equation, the dosage of reactants, and the optimal reaction temperature Ty;

[0034] Put a preset dosage of reactants into the continuous pipeline, and perform the first temperature measurement, collect the real-time data of each temperature sensor and take the average value as the initial reaction temperature T0;

[0035] Trigger the reaction conditions, carry out the reaction, and monitor the real-time temperature Ts of the reactants inside the continuous pipeline in real time. When the real-time temperature Ts = Ty, start the cooling jacket to cool down, so as to keep the real-time temperature of the reactants inside the continuous pipeline within the temperature range (Ty - 1.75K, Ty + K), where K is a preset temperature margin;

[0036] When, as the reaction progresses, the real-time temperature Ts ≤ Ty - 1.75K, continue to cool the continuous pipeline through the cooling jacket, and when the real-time temperature Ts = T0, partially close the cooling jacket. The partial closing means stopping the heat exchange between the cooling jacket and the continuous pipeline, and still retaining the heat exchange between the cooling jacket and the heat exchange water tank until the cooling medium in the cooling jacket returns to the initial heat exchange temperature and is completely closed;

[0037] Calculate the reaction heat Qf according to the formula. The specific formula is: Qf = cmΔt, where c represents the specific heat capacity of the cooling water, m represents the mass of the cooling water in the cooling water tank, and Δt represents the temperature rise of the cooling water in the cooling water tank.

[0038] It should be noted that in the common reaction heat testing methods, the reaction heat released during the reaction process is calculated based on the temperature change inside the reactants or the reaction system. However, in this case, in order to accurately measure the temperature change brought about by the reaction heat, it is necessary to ensure as little heat exchange as possible between the reaction system and the outside world; therefore, in some cases where the reaction is relatively violent, a large amount of reaction heat is generated, resulting in a rapid increase in temperature, and the excessive temperature will further accelerate the reaction rate, generating more reaction heat, which is relatively dangerous;

[0039] Therefore, in the solution of the present invention, the reaction process is placed in a continuous pipeline, and the inside of the pipeline is in continuous flow, that is, the common U-shaped or circular pipeline, and the material circulation flow is realized by connecting the head and the tail; therefore, the present invention is mainly aimed at the reaction heat test method for the solution reaction system, and for the reaction system without fluidity or with poor fluidity or the product will precipitate and condense, the effect is poor;

[0040] In the present invention, through the externally provided cooling jacket, the temperature change of the continuous pipeline during the reaction process can be controlled, so as to control the reaction rate, making it safer, and effectively avoiding the generation of side reactions or by-products; and because there will also be corresponding material changes during the reaction process, such as the generation of gas, etc., the continuous pipeline in the present invention can effectively increase the reaction safety; secondly, while ensuring the optimal reaction temperature in the present invention, the heat generated by the reaction is transferred to the water tank through heat exchange, so as to more conveniently calculate the heat released during the reaction process.

[0041] In a preferred embodiment of the present invention, the specific steps for calculating the real-time temperature Ts are as follows:

[0042] Drive the continuous pipeline to rotate or swing to ensure uniform mixing of the reactants inside the continuous pipeline;

[0043] Obtain the real-time measurement data of a plurality of temperature sensors, and when the difference between any two real-time measurement data is less than or equal to the preset measurement error, take the average value of the plurality of real-time measurement data as the real-time temperature Ts of the reactants inside the continuous pipeline.

[0044] In a preferred embodiment of the present invention, when the difference between any two real-time measurement data among the real-time measurement data of a plurality of temperature sensors is greater than the preset measurement error, the real-time measurement data of the temperature sensors are re-obtained.

[0045] In a preferred embodiment of the present invention, there is also a standby water tank. After the cooling jacket is partially closed, when the temperature of the cooling medium in the cooling jacket is greater than the initial heat exchange temperature and less than or equal to (T'+t), the heat exchange between the cooling jacket and the heat exchange water tank is closed, and the heat exchange between the cooling jacket and the standby water tank is carried out, where T' represents the temperature of the cooling water in the cold water tank, and t represents the preset heat exchange temperature difference.

[0046] The standby water tank is used as an alternative to the cooling water tank, and its function is the same as that of the cooling water tank. The purpose of setting the standby water tank is to prevent the cooling water tank from not meeting the heat exchange requirements when the reaction heat is too large.

[0047] In a preferred embodiment of the present invention, when a spare water tank is connected to the cooling jacket until the cooling medium in the cooling jacket returns to the initial heat exchange temperature, the calculation formula for the reaction heat is: Qf = c(mΔt + m'Δt'), where m' represents the mass of the cooling water in the spare water tank, and Δt represents the temperature rise of the cooling water in the spare water tank.

[0048] In a preferred embodiment of the present invention, the cooling jacket is provided with multiple circuits, including a reaction heat exchange circuit, a cooling circuit, a spare heat exchange circuit, and a spare cooling circuit. In the reaction heat exchange circuit, the cooling jacket exchanges heat between the continuous pipeline and the cooling water tank simultaneously; in the cooling circuit, the cooling jacket exchanges heat only with the cooling water tank; in the spare heat exchange circuit, the cooling jacket exchanges heat between the continuous pipeline and the spare water tank simultaneously; in the spare cooling circuit, the cooling jacket exchanges heat only with the spare water tank.

[0049] In a preferred embodiment of the present invention, when the temperature difference between the cooling water in the cooling water tank and the continuous pipeline is less than a preset value, the heat exchange circuit is switched to the spare heat exchange circuit, and after partially closing the cooling jacket, heat exchange is carried out through the spare cooling circuit.

[0050] A continuous pipeline reaction heat test system includes a continuous pipeline serving as a reaction vessel and a cooling jacket provided on the continuous pipeline, and a plurality of temperature sensors are provided on the continuous pipeline, and a heat exchange water tank is also provided on the cooling jacket, including:

[0051] Initialization module: Obtain reaction data, where the reaction data includes a reaction equation, reactant dosage, and the optimal reaction temperature Ty;

[0052] Pretreatment module: Put a preset dosage of reactants into the continuous pipeline, conduct the first temperature measurement, collect the real-time data of each temperature sensor, and take the average value as the initial reaction temperature T0;

[0053] Reaction control module: Trigger reaction conditions, conduct the reaction, and monitor the real-time temperature Ts of the reactants inside the continuous pipeline in real time. When the real-time temperature Ts = Ty, start the cooling jacket to cool down, so as to keep the real-time temperature of the reactants inside the continuous pipeline within the temperature range (Ty - 1.75K, Ty + K), where K is a preset temperature margin;

[0054] Reaction heat calculation module: When, as the reaction proceeds, the real-time temperature Ts ≤ Ty - 1.75K, the continuous pipeline is further cooled through the cooling jacket. When the real-time temperature Ts = T0, the cooling jacket is partially closed. The partial closure means stopping the heat exchange between the cooling jacket and the continuous pipeline, while still retaining the heat exchange between the cooling jacket and the heat exchange water tank, until the cooling medium in the cooling jacket returns to the initial heat exchange temperature and is completely closed.

[0055] Calculate the reaction heat Qf according to the formula. The specific formula is: Qf = cmΔt, where c represents the specific heat capacity of the cooling water, m represents the mass of the cooling water in the cooling water tank, and Δt represents the temperature rise of the cooling water in the cooling water tank.

[0056] The above has described a specific embodiment of the present invention in detail, but the described content is only a preferred embodiment of the present invention and cannot be considered as limiting the scope of implementation of the present invention. Any equivalent changes and improvements made within the scope of the application of the present invention shall still fall within the scope covered by the patent of the present invention.

Claims

1. A continuous pipeline reaction heat testing method, comprising a continuous pipeline serving as a reaction vessel and a cooling jacket provided on the continuous pipeline, and a plurality of temperature sensors are provided on the continuous pipeline, and a heat exchange water tank is further provided on the cooling jacket, characterized in that, It includes the following steps: Obtain reaction data, where the reaction data includes reaction equations, reactant dosages, and the optimal reaction temperature Ty; Put a preset dosage of reactants into the continuous pipeline, conduct the first temperature measurement, collect the real-time data of each temperature sensor, and take the average value as the initial reaction temperature T0; Trigger the reaction conditions, conduct the reaction, and monitor the real-time temperature Ts of the reactants inside the continuous pipeline in real time. When the real-time temperature Ts = Ty, start the cooling jacket to cool down, so as to keep the real-time temperature of the reactants inside the continuous pipeline within the temperature range (Ty - 1.75K, Ty + K), where K is the preset temperature margin; When, as the reaction progresses, the real-time temperature Ts ≤ Ty - 1.75K, continue to cool the continuous pipeline through the cooling jacket. When the real-time temperature Ts = T0, the cooling jacket is partially closed. The partial closure means stopping the heat exchange between the cooling jacket and the continuous pipeline, and still retaining the heat exchange between the cooling jacket and the water tank for heat exchange, until the cooling medium in the cooling jacket returns to the initial heat exchange temperature and is completely closed; Calculate the reaction heat Qf according to the formula. The specific formula is: Qf = cmΔt, where c represents the specific heat capacity of the cooling water, m represents the mass of the cooling water in the cooling water tank, and Δt represents the temperature rise of the cooling water in the cooling water tank.

2. The continuous pipeline reaction heat testing method according to claim 1, wherein, The specific steps for calculating the real-time temperature Ts are as follows: Drive the continuous pipeline to rotate or swing to ensure uniform mixing of the reactants inside the continuous pipeline; Obtain the real-time measurement data of several temperature sensors. When the difference between any two real-time measurement data is less than or equal to the preset measurement error, take the average value of the several real-time measurement data as the real-time temperature Ts of the reactants inside the continuous pipeline.

3. A continuous pipeline reaction heat testing method according to claim 2, characterized in that, When, among the real-time measurement data of several temperature sensors, the difference between any two real-time measurement data is greater than the preset measurement error, re-obtain the real-time measurement data of the temperature sensors.

4. The continuous pipeline reaction heat testing method according to claim 1, characterized in that It also includes a standby water tank. After the cooling jacket is partially closed, when the temperature of the cooling medium in the cooling jacket is greater than the initial heat exchange temperature and less than or equal to (T' + t), close the heat exchange between the cooling jacket and the water tank for heat exchange, and conduct heat exchange between the cooling jacket and the standby water tank, where T' represents the temperature of the cooling water in the cold water tank, and t represents the preset heat exchange temperature difference; After the cooling jacket is connected to the standby water tank until the cooling medium in the cooling jacket returns to the initial heat exchange temperature, the calculation formula for the reaction heat is: Qf = c(mΔt + m'Δt'), where m' represents the mass of the cooling water in the standby water tank, and Δt' represents the temperature rise of the cooling water in the standby water tank.

5. A continuous pipeline reaction heat testing method according to claim 4, characterized in that, The described cooling jacket is provided with multiple circuits, including a reaction heat exchange circuit, a cooling circuit, a standby heat exchange circuit, and a standby cooling circuit. In the reaction heat exchange circuit, the cooling jacket exchanges heat between the continuous pipeline and the cooling water tank simultaneously; in the cooling circuit, the cooling jacket exchanges heat only with the cooling water tank; in the standby heat exchange circuit, the cooling jacket exchanges heat between the continuous pipeline and the standby water tank simultaneously; in the standby cooling circuit, the cooling jacket exchanges heat only with the standby water tank.

6. The method for testing the reaction heat of a continuous pipeline according to claim 5, characterized in that, When the temperature difference between the cooling water in the cooling water tank and the continuous pipeline is less than a preset value, switch the heat exchange circuit to the standby heat exchange circuit, and after partially closing the cooling jacket, perform heat exchange through the standby cooling circuit.

7. A continuous pipeline reaction heat testing system, comprising a continuous pipeline serving as a reaction vessel and a cooling jacket provided on the continuous pipeline, and a plurality of temperature sensors are provided on the continuous pipeline, and a heat exchange water tank is further provided on the cooling jacket, characterized in that, It includes: Initialization module: Obtain reaction data, where the reaction data includes a reaction equation, the dosage of reactants, and the optimal reaction temperature Ty; Pretreatment module: Put a preset dosage of reactants into the continuous pipeline, and perform the first temperature measurement. Collect the real-time data of each temperature sensor and take the average value as the initial reaction temperature T0; Reaction control module: Trigger the reaction conditions, carry out the reaction, and monitor the real-time temperature Ts of the reactants inside the continuous pipeline in real time. When the real-time temperature Ts = Ty, start the cooling jacket to cool down, so as to keep the real-time temperature of the reactants inside the continuous pipeline within the temperature range (Ty - 1.75K, Ty + K), where K is a preset temperature margin; Reaction heat calculation module: When the real-time temperature Ts ≤ Ty - 1.75K during the reaction, continue to cool down the continuous pipeline through the cooling jacket. When the real-time temperature Ts = T0, the cooling jacket is partially closed. The partial closing means stopping the heat exchange between the cooling jacket and the continuous pipeline, and still retaining the heat exchange between the cooling jacket and the heat exchange water tank until the cooling medium in the cooling jacket returns to the initial heat exchange temperature and then is completely closed; Calculate the reaction heat Qf according to the formula. The specific formula is: Qf = cmΔt, where c represents the specific heat capacity of the cooling water, m represents the mass of the cooling water in the cooling water tank, and Δt represents the temperature rise of the cooling water in the cooling water tank.

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