Portable device for measuring chemical reaction heat and measuring method

Abstract

The invention relates to a portable chemical reaction heat measuring device and a measuring method.The portable chemical reaction heat measuring device comprises a shell, a temperature control and calorimetric device, a weight testing device, a sample injection structure, a control structure and a leakage-proof connector, the temperature control and calorimetric device comprises a temperature sensor, a testing container and a reference container, and the testing container and the reference container are arranged in the shell in parallel; the temperature sensor measures temperature changes and sends data to the control structure, the weight testing device is arranged below the testing container, monitors and records weight changes of materials and sends data to the control structure, the sample injection structure is communicated with the testing container through a leakage-proof connector and provides samples, and the pressure sensor is arranged on the outer side of the testing container and used for detecting the temperature changes of the materials. And a reaction heat calculation program is also arranged in the control structure. By adopting the calorimetric equipment, the reaction heat test can be directly carried out on the production site, and by virtue of a specific sample introduction structure and a weighing system, not only can materials be prevented from being contacted with the outside, but also the input material quantity can be accurately weighed.

Description

Technical Field

[0001] This invention relates to the field of chemical process reaction heat measurement technology, specifically to a portable device and method for measuring the heat of chemical reactions. Background Technology

[0002] Fine chemicals are a strategic focus of my country's chemical industry development. Most fine chemical reactions are exothermic, and thermal runaway during these reactions can cause immense damage to human life, property, and the environment. Measuring the heat generated during a reaction is a crucial parameter for assessing the hazard of the process and a vital reference for process design and equipment capacity. However, current calorimetric technologies and equipment are primarily concentrated in laboratory environments, often encountering problems such as inaccurate measurements, high testing risks, or even the inability to measure materials that are easily perishable or prone to leakage during transportation.

[0003] Fine chemical reactants are diverse in type and state, and some materials (especially intermediates) are unstable (easily decomposed, react with air, etc.) or highly toxic. These properties limit the transportation distance of materials, making it impossible to transport samples to laboratories outside or even within the company for testing. Existing testing equipment is mainly used for testing in laboratory environments and cannot test reactions involving the above-mentioned samples, or the test results are significantly biased. Reaction calorimetry apparatus (CN209222095U) and a method and apparatus for determining the heat of chemical reaction (CN1869620A) respectively introduce reaction calorimetry testing devices based on laboratory environments, but neither device can solve the risks of deterioration of thermally unstable materials and leakage of toxic gases during transportation.

[0004] Therefore, the problems of limited application scenarios, poor applicability, lack of convenience, and poor sealing in the existing technology of reaction heat measurement are issues that urgently need to be addressed by those skilled in the art. Summary of the Invention

[0005] In view of the problems existing in the prior art regarding chemical reactions involving materials that are difficult to sample in industrial production, difficult to transport, react with air, or are flammable, explosive, or highly toxic, as well as other problems that are difficult to test reaction heat in the laboratory, the purpose of this invention is to provide a chemical reaction calorimetry parameter device and method that can measure reaction heat on-site in enterprises and is suitable for production sites.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a portable device for measuring the heat of chemical reaction, comprising a shell, a temperature control and calorimetry device, a weight testing device, a sample introduction structure, a control structure, and a leak-proof interface. The temperature control and calorimetry device includes a temperature sensor, a test container, and a reference container. The test container and the reference container are arranged parallel to each other within the shell. The temperature sensor measures the temperature changes within the test container and the reference container and sends the temperature change data to the control structure. The weight testing device is located below the test container and is used to monitor and record the weight changes of the material within the test container and send the weight change data to the control structure. The sample introduction structure is connected to the test container through the leak-proof interface and provides a sample to the temperature control and calorimetry device. A pressure sensor is provided on the outside of the test container. The control structure also includes a reaction heat calculation program.

[0007] The aforementioned portable device for measuring the heat of chemical reaction further includes a stir bar, which is disposed at the bottom of the test container and the reference container.

[0008] The aforementioned portable device for measuring the heat of chemical reaction includes a sample injection structure comprising a sample injection motor, a sample injection chamber, a sample inlet, a sample outlet, a piston, and a push rod. A push rod hole is provided at the bottom of the sample injection chamber. The piston is disposed within the sample injection chamber. One end of the push rod is connected to the piston, and the other end passes through the push rod hole and is connected to the output end of the sample injection motor. The sample injection motor drives the piston to reciprocate within the sample injection chamber. The sample inlet and sample outlet are located on the chamber wall above the piston. A sample collection port is provided on the outer side of the sample inlet, and the sample outlet is connected to the leak-proof interface.

[0009] The aforementioned portable device for measuring the heat of chemical reaction further includes two one-way valves in the sample injection structure. The one-way valves are respectively located at the sample inlet and the sample outlet. Under the action of the piston and the one-way valves, when the piston moves downward, the sample enters the sample injection chamber through the sample inlet. When the piston moves upward, the sample leaves the sample injection chamber through the sample outlet.

[0010] The aforementioned portable device for measuring the heat of chemical reaction includes a leak-proof interface comprising a female interface and a female interface. The female interface is fitted inside the female interface, the female interface is connected to the sample outlet, and the female interface is connected to the test container.

[0011] The aforementioned portable device for measuring the heat of chemical reaction includes a female port comprising a female port shell, a female port tube, an annular cavity, a female port isolator, a female port spring, and a female port fixing buckle. The female port tube is disposed inside the female port shell and has a first sample port. The top end of the female port tube is closed, and the bottom end is connected to the sample outlet. The annular cavity is formed between the female port shell and the female port tube. The female port isolator is sleeved on the outside of the female port tube and moves up and down within the annular cavity. The female port spring is disposed below the female port isolator. The female port fixing buckle is disposed inside the female port shell to limit the position of the female port isolator.

[0012] The aforementioned portable device for measuring the heat of chemical reaction includes an interface sub-port comprising a sub-port outer shell, an inner sub-port tube, an outer sub-port tube, a sub-port isolator, a sub-port spring, and a sub-port tubing support. The sub-port outer shell is inserted into the annular cavity. The inner and outer sub-port tubes are disposed inside the sub-port outer shell. The inner sub-port tube has a sub-port hole, which communicates with the outside through its top and is closed at its bottom. The outer sub-port tube is disposed on the other side of the sub-port hole and is connected to a test container. The sub-port isolator is slidably fitted inside the inner sub-port tube to open and close the sub-port hole. The sub-port spring is disposed between the sub-port isolator and the bottom wall of the inner sub-port tube. The sub-port tubing support is disposed between the inner and outer sub-port tubes to fix the inner sub-port tube.

[0013] The aforementioned portable device for measuring the heat of chemical reaction further includes a differential thermal amplifier, a power compensator, a data acquisition unit, and a thermocouple cold junction compensator in its control structure. When the sample in the test container reacts and releases heat, the temperature of the test container is higher than that of the reference container. The thermocouple in the temperature control and calorimetry device generates a temperature difference potential, which is amplified by the differential thermal amplifier and then sent to the power compensator. The control structure automatically lowers the temperature of the test container based on the data feedback from the data acquisition unit, so that the temperature difference between the test container and the reference container approaches zero. The thermocouple cold junction compensation device is used to eliminate the error caused by the temperature difference between the thermocouple and the test container.

[0014] A test method for a portable device for measuring the heat of chemical reaction includes the following steps: Step 1: Assemble the portable device for measuring the heat of chemical reaction as described in any of the above items, connect the temperature control and calorimetry device to the control structure using a data cable, connect the sample injection structure to the nitrogen gas source, and purge the pipeline with nitrogen. Step 2: Connect the injection device to the sample one pipeline, control the injection device to pump the sample one into the pipeline for rinsing, after rinsing is completed, control the injection device to stop pumping, close the female port and wipe the interface dry; Step 3: Connect the injection structure and the test container, control the injection structure to pump in sample one, when the weight test structure detects that sample one is close to the limit value, it sends a signal to the control structure, the control structure controls the injection structure to slow down the injection speed, and accurately add the material. After the material is added, disconnect the injection structure from the test container. Step 4: Replace the injection structure and the tubing connected to the test container, reconnect them, and connect the newly connected injection structure to the nitrogen source, and purge the tubing with nitrogen. Step 5: Adjust the temperature control and calorimeter to the initial temperature using the control structure; Step 6: Connect the injection structure from Step 4 to the sample two pipeline, control the injection structure to pump the sample two into the pipeline for rinsing, after rinsing is completed, control the injection structure to stop pumping, close the female port and wipe the interface dry. Step 7: Connect the injection structure and the test container, control the injection structure to pump in sample two. When the weight test structure detects that sample two is close to the limit value, it sends a signal to the control structure. The control structure controls the injection structure to slow down the injection speed and accurately add the material. After the material is added, disconnect the injection structure from the test container. Step 8: Adjust the temperature in the temperature control and calorimeter to the reaction temperature using the control structure, control the heating time, and obtain the heat flow in the test container and reference container respectively through temperature sensors. Step 9: Perform reaction heat calculation using the reaction heat calculation program of the control structure to obtain the heat flow of the reaction.

[0015] In the above-described test method for a portable device for measuring the heat of chemical reaction, step 9 involves subtracting the heat flow of the reference container from the heat flow of the test container to obtain the heat flow of the reaction. The calculation formula is as follows: ΔW = dQs / dt - dQr / dt = dH / dt, where dQs / dt represents the heat supplied to the test container per unit time, dQr / dt represents the heat supplied to the reference container per unit time, and dH / dt represents the rate of change of enthalpy.

[0016] The beneficial effects of this portable device and method for measuring the heat of chemical reaction are as follows: This invention uses calorimetry equipment, allowing for direct on-site testing of the heat of reaction. Through a specific sample introduction structure and weighing system, it not only avoids external contact between the material and the environment but also accurately weighs the amount of material input. This significantly improves the accuracy and practicality of the test, especially for unstable reaction raw materials. Furthermore, this calorimetry equipment requires a small amount of material during the reaction process, greatly enhancing safety during testing, particularly for highly hazardous reactions.

[0017] The device allows for on-site sampling and direct determination of the heat of reaction using its integrated sample inlet tubing, electronic balance, and calorimetric system. The tubing connections and other components are well-sealed, effectively preventing the leakage of toxic substances or the entry of airborne particles that could affect the accuracy of the reaction measurements. The detachable tubing assembly ensures accurate feed rates and prevents premature reactions within the tubing. Furthermore, the device is compact, portable, and not limited by testing location. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic diagram illustrating the working principle of the chemical reaction calorimeter of the present invention; Figure 3 This is a left view of the sample introduction structure of the present invention; Figure 4 This is a front view of the sample inlet chamber structure of the present invention; Figure 5 This is a schematic diagram of the closed state structure of the female interface of the present invention; Figure 6 This is a schematic diagram of the female interface port of the present invention in the open state. Figure 7 This is a schematic diagram of the sealing state structure of the interface sub-port of the present invention; Figure 8 This is a schematic diagram of the interface sub-port open state structure of the present invention; Figure 9 This is a schematic diagram of the three-dimensional structure of the female interface of the present invention; Figure 10 This is a schematic diagram of the three-dimensional structure of the interface sub-port of the present invention; Figure 11 This is a schematic diagram of the connection between the female / female port pipeline and the female / female port isolator of the present invention.

[0019] Figure reference numerals: 1. Temperature control and calorimetry device; 2. Test container; 3. Reference container; 4. Stirrer; 5. Weight testing device; 6. Pressure sensor; 7. Sample injection structure; 71. Display screen; 72. Operation panel; 73. Battery; 74. Sample injection pump motor; 75. Sample injection pump piston rod; 76. Sample injection chamber; 77. First one-way valve; 78. Sample inlet; 79. Second one-way valve; 710. Sample outlet; 8. Sample collection port; 9. Control structure; 10. Leak-proof interface; 11. Female connector. 101 outer casing, 102 female port pipe, 103 female port isolator, 104 female port spring, 105 female port fixing buckle, 106 female port outer casing, 107 female port inner tube, 108 female port outer tube, 109 female port isolator, 1010 female port spring, 1011 female port pipe support, 1012 circular hole, 1013 cylindrical hole, 11 differential thermal amplifier, 12 data logger, 13 power compensator, 14 thermocouple cold junction compensation device. Detailed Implementation

[0020] To enable those skilled in the art to better understand the technical solution and objectives of the present invention, the technical solution and objectives of the present invention will be described below in conjunction with specific embodiments and accompanying drawings.

[0021] Example 1 like Figure 1-10 As shown, this embodiment provides a chemical reaction calorimeter suitable for production sites. It is small in size, easy to operate, and portable. The testing temperature range of this chemical reaction calorimeter is room temperature to 200°C, with a maximum pressure resistance of 5 bar. It is suitable for most common liquid-liquid reactions, liquid-solid reactions, gas-liquid reactions, and gas-solid reactions.

[0022] The main body of this chemical reaction calorimeter is the temperature control and calorimeter device 1. The temperature control and calorimeter device 1 has a built-in sensitive three-dimensional temperature sensor. The temperature control and calorimeter device contains a test container 2 and a reference container 3. The test container 2 is divided into a glass test container with normal pressure and an alloy test container with high pressure, with a volume of 10mL. The high pressure test container can withstand a maximum pressure of 5bar. The temperature sensor can sensitively detect the changes in the test container and the reference container to obtain the changes in heat flow for endothermic and exothermic reactions.

[0023] Stirrers 4, coated with a corrosion-resistant polymer material, are placed in test container 2 and reference container 3. A weight testing device 5, located at the bottom of the test container, can monitor and record the weight changes of the materials in the test container in real time, allowing for convenient control of the feeding amount and effectively reducing the risk of adding hazardous materials after external weighing. The top cover of test container 2 has two channels connecting to the outside. One channel connects to a pressure sensor 6, which can monitor pressure changes during the reaction process. The other channel connects to the sample inlet structure 7 via a self-sealing, leak-proof interface 10. A sampling port 8 is located on the outside of the sample inlet structure. The entire pathway—test container, sample inlet structure, and sampling port—is sealed and airtight.

[0024] The sample introduction structure 7 has a display screen 71 and an operation panel 72 fixed on the front, a rechargeable lithium battery module 73 at the bottom, and a sample introduction motor 74 and a detachable sample introduction chamber 76 at the upper rear. The entire sample introduction structure is well-sealed, providing dustproof, waterproof, and dirt-proof capabilities. The top of the sample introduction chamber 76 is connected to the sample inlet 78 via a first one-way valve 77 (inlet one-way valve), and the upper right side of the sample introduction chamber 76 is connected to the sample outlet 710 via a second one-way valve 79 (outlet one-way valve). The sample can only flow in one direction in the inlet-sample chamber-sample outlet passage. The sample introduction chamber has a T-shaped piston push rod 75, the piston cross-section at the top of the push rod is perfectly matched with the cross-section of the sample introduction chamber, and the rod is connected to the sample pump motor 74 through a push rod hole at the bottom. Under the action of the sample pump motor, the piston pusher moves longitudinally in the sample injection chamber. When the piston pusher moves downward, the volume of the sample injection chamber increases, the internal pressure decreases, and the sample is drawn into the sample injection chamber from the injection port. When the piston pusher moves upward, the volume of the sample injection chamber decreases, the internal pressure increases, and the sample leaves the sample injection chamber from the outlet. To facilitate cleaning or the addition of different samples, the sample inlet 78, sample injection chamber 76, sample outlet 710, and piston pusher 75 are designed to be detachable. The piston pusher 75 is not fixedly connected to the sample injection motor 74 and can be directly pulled out from the sample injection motor.

[0025] When replacing the injection line, the injection line needs to be reconnected to the inlet on the cover of the test container 2. To prevent air from entering or toxic substances from escaping during the connection process, a leak-proof interface 10 that is easy to plug and unplug is specially designed. The female port of the interface is connected to the injection structure, and the female port of the interface is connected to the top cover of the test container. The outer layer of the female port is a metal female port shell 101. Inside the shell is a female port tube 102 for sample flow. There is an annular cavity between the outer wall and the tube. The top of the tube is sealed. There are several circular holes 1012 on the top side wall. The sample can enter the annular cavity through the circular holes and then flow out of the female port. A tubular female port isolator 103 is installed in the annular cavity. The female port isolator is fitted on the top of the female port tube. The tangential surface of the female port isolator in contact with the top of the female port tube has a certain angle. Under the action of internal pressure or spring pressure, the isolator can keep the tube sealed. There are several female port springs 104 at the lower end of the female port isolator. The other end of the springs presses on the base of the female port shell. When not connected, the isolator 103, under the action of the spring, is at the top of the annular cavity, which can cover the circular hole of the female port pipeline and prevent the sample from flowing out. When connected, the female port isolator is slid to the bottom of the annular cavity by external force, exposing the circular hole in the pipeline, and the sample flows out. The female port housing is provided with a female port fixing bayonet 105 on the inner side, which is used to fix the female port when connected.

[0026] The outer layer of the connector is a metal outer shell 106. Inside the outer shell are inner and outer tubes. The inner tube 107 connects to the outside via its top. The inner tube has several circular holes in its wall. On the other side of these holes is the outer tube 108, which connects to the tube at the bottom of the connector. A columnar connector isolator 109 is located inside the inner tube. A connector spring 1010 is located at the lower end of the isolator. The outer shell is inserted into an annular cavity. The inner and outer tubes are located inside the outer shell. The inner tube has a connector hole, connecting to the outside via its top and being closed at the bottom. The outer tube is located on the other side of the connector hole and connects to the test container. The isolator slides inside the inner tube to open and close the connector hole. The sub-port spring is positioned between the sub-port isolator and the bottom wall of the sub-port inner tube. The contact surface between the sub-port isolator and the top of the sub-port pipe has a certain angle. Under the action of internal pressure or spring pressure, it can keep the isolator and the pipe sealed. When not connected, the sub-port isolator is located at the top of the sub-port inner tube under the action of the sub-port spring, isolating the inner tube from the outside. When the sub-port is connected, the sub-port isolator moves to the lower part of the sub-port inner tube, at which time the sub-port outer tube can communicate with the outside through the circular hole. The lower middle part of the sub-port outer tube is provided with a sub-port pipe support 1011, which connects the sub-port inner tube and the sub-port outer tube and provides support for the sub-port inner tube. The sub-port pipe support has columnar holes 1013, through which liquid entering from the outside can enter the pipe at the bottom of the sub-port.

[0027] The working principle of the chemical reaction calorimeter suitable for production sites is the power compensation method. Maintaining the test container 2 and the reference container 3 at the same temperature, the energy difference required between the two containers to meet this condition is measured and directly output as the signal ΔQ. When the sample reaction in the test container 2 releases heat, the temperature of the test container 2 is higher than that of the reference container 3. The thermocouples in the temperature control and calorimetry device generate a temperature difference potential, which is amplified by the differential thermal amplifier 11 controlled by the control structure and then sent to the power compensator 13. The control structure automatically lowers the temperature of the test container based on the data feedback from the data acquisition unit 12, making the temperature difference ΔT between the test container and the reference container approach zero. The thermocouple cold junction compensation device 14 is used to eliminate the error caused by the temperature difference between the thermocouple and the testing device.

[0028] The energy difference ΔW (dH / dt) required to maintain the test container and the reference container at the same temperature, as measured by this chemical reaction calorimeter, reflects the change in the enthalpy of the reaction. The calculation formula is shown below: ΔW = dQs / dt - dQr / dt = dH / dt dQs / dt: Heat delivered to the test container per unit time; dQr / dt: Heat supplied to the reference container per unit time; dH / dt: Enthalpy change rate.

[0029] Example 2 like Figure 1-10 As shown, a portable device for measuring the heat of chemical reaction includes a housing, a temperature control and calorimetry device, a weight testing device, a sample injection structure, a control structure, and a leak-proof interface. The temperature control and calorimetry device includes a temperature sensor, a test container, and a reference container. The test container and the reference container are arranged parallel to each other inside the housing. The temperature sensor measures the temperature change inside the test container and the reference container and sends the temperature change data to the control structure. A pressure sensor is provided on the outside of the test container.

[0030] Furthermore, to facilitate sample mixing, the temperature control and calorimetry device also includes a stir bar, which is located at the bottom of the test container and the reference container.

[0031] The weight testing device is located below the test container to monitor and record the weight changes of the material inside the test container and send the weight change data to the control structure.

[0032] The sample injection structure is connected to the test container through a leak-proof interface and provides samples to the temperature control and calorimetry device. The sample injection structure includes a sample injection motor, a sample injection chamber, a sample inlet, a sample outlet, a piston, and a push rod. A push rod hole is provided at the bottom of the sample injection chamber. The piston is located in the sample injection chamber. One end of the push rod is connected to the piston, and the other end passes through the push rod hole and is connected to the output end of the sample injection motor. The sample injection motor drives the piston to reciprocate in the sample injection chamber. The sample inlet and sample outlet are located on the chamber wall of the sample injection chamber above the piston. A sample collection port is provided on the outside of the sample inlet, and the sample outlet is connected to the leak-proof interface.

[0033] Furthermore, to control the flow direction of the sample, the injection structure also includes two one-way valves, which are respectively located at the injection port and the outlet. Under the action of the piston and the one-way valves, when the piston moves downward, the sample enters the injection chamber through the injection port. When the piston moves upward, the sample leaves the injection chamber through the outlet.

[0034] The leak-proof interface includes a female interface and a female interface. The female interface is fitted inside the female interface. The female interface is connected to the sample outlet, and the female interface is connected to the test container.

[0035] The female interface includes a female interface shell, a female interface tube, an annular cavity, a female interface isolator, a female interface spring, and a female interface fixing buckle. The female interface tube is located inside the female interface shell and has a first sample port. The top of the female interface tube is closed, and the bottom end is connected to the sample outlet. An annular cavity is formed between the female interface shell and the female interface tube. The female interface isolator is sleeved on the outside of the female interface tube and moves up and down within the annular cavity. The female interface spring is located below the female interface isolator, and the female interface fixing buckle is located inside the female interface shell to limit the position of the female interface isolator.

[0036] The interface includes an outer shell, an inner tube, an outer tube, an isolator, a spring, and a pipe support. The outer shell is inserted into an annular cavity. The inner and outer tubes are located inside the outer shell. The inner tube has an opening that connects to the outside through its top and is closed at the bottom. The outer tube is located on the other side of the opening and is connected to the test container. The isolator is slidably fitted inside the inner tube to open and close the opening. The spring is located between the isolator and the bottom wall of the inner tube. The pipe support is located between the inner and outer tubes to fix the inner tube.

[0037] The control structure also includes a reaction heat calculation program, a differential thermal amplifier, a power compensator, a data acquisition unit, and a thermocouple cold junction compensator. When the sample reacts and releases heat in the test container, the temperature of the test container is higher than that of the reference container. The thermocouples in the temperature control and calorimetry device will generate a temperature difference potential, which is amplified by the differential thermal amplifier and sent to the power compensator. The control structure automatically reduces the temperature of the test container based on the data feedback from the data acquisition unit, so that the temperature difference between the test container and the reference container approaches zero. The thermocouple cold junction compensation device is used to eliminate the error caused by the temperature difference between the thermocouple and the test container.

[0038] Example 3 A test method for a portable device for measuring the heat of chemical reaction includes the following steps.

[0039] Step 1: Assemble the portable device for measuring the heat of chemical reaction as described in Examples 1 and 2. Connect the temperature control and calorimetry device to the control structure using a data cable. Connect the sample injection structure to the nitrogen gas source and purge the pipeline with nitrogen.

[0040] Step 2: Connect the injection device to the sample line, control the injection device to pump the sample into the line for rinsing, after rinsing, control the injection device to stop pumping, close the female port and wipe the interface dry.

[0041] Step 3: Connect the injection structure and the test container. Control the injection structure to pump in sample one. When the weight test structure detects that sample one is close to the limit value, it sends a signal to the control structure. The control structure controls the injection structure to slow down the injection speed for precise feeding. After feeding is completed, disconnect the injection structure from the test container.

[0042] Step 4: Replace the injection structure and the tubing connected to the test container, reconnect them, connect the newly connected injection structure to the nitrogen source, and purge the tubing with nitrogen.

[0043] Step 5: Use the control structure to adjust the temperature control and calorimeter to the initial temperature.

[0044] Step 6: Connect the injection structure from Step 4 to the sample two pipeline, control the injection structure to pump the sample two into the pipeline for rinsing, after rinsing is completed, control the injection structure to stop pumping, close the female port and wipe the interface dry.

[0045] Step 7: Connect the injection structure and the test container. Control the injection structure to pump in sample two. When the weight test structure detects that sample two is close to the limit value, it sends a signal to the control structure. The control structure controls the injection structure to slow down the injection speed and accurately add the material. After the material is added, disconnect the injection structure from the test container.

[0046] Step 8: Adjust the temperature in the temperature control and calorimeter to the reaction temperature using the control structure, control the heating time, and obtain the heat flow in the test container and reference container through temperature sensors.

[0047] Step 9: Perform reaction heat calculation using the reaction heat calculation program of the control structure to obtain the heat flow of the reaction.

[0048] Specifically, the heat flux of the reaction is obtained by subtracting the heat flux of the reference container from the heat flux of the test container. The calculation formula is as follows: ΔW = dQs / dt - dQr / dt = dH / dt, where dQs / dt represents the heat supplied to the test container per unit time, dQr / dt represents the heat supplied to the reference container per unit time, and dH / dt represents the rate of change of enthalpy.

[0049] Example 4 This embodiment and embodiments 5-11 are specific applications of the portable device for measuring the heat of chemical reaction described in embodiments 1 and 2 and the measurement method described in embodiment 3. This embodiment is used to prepare an imine compound (Grignard reagent) by reacting cyanopyridine with ethyl magnesium chloride (Grignard reagent), specifically including...

[0050] Step 1: Assemble and connect the components of the portable device for measuring the heat of chemical reaction according to the overall schematic diagrams of Examples 1 and 2. Place the clean glass test container 2 and reference container 3 on the weight testing device 5 in the temperature control and calorimetry device 1, and add the stir bar 4 into the test container 2. Connect the pressure sensor 6 and the interface of the leak-proof interface 10 to the top of the test container 2, respectively. The female interface of the leak-proof interface is connected to the sample outlet of the sample inlet structure 7, and the sample inlet of the sample inlet structure 7 is connected to the sample collection port 8. The temperature control and calorimetry device is connected to the central control system of the control structure 9 via a data cable.

[0051] Step 2: Connect sample collection port 8 to the nitrogen source. Control the injection structure 7 to continuously pump nitrogen into the testing device along the pipeline, purging air from the pipeline and testing container 2. The nitrogen purging time is 10 minutes. After purging, control the injection structure 7 to stop pumping and disconnect the collection port 8 from the nitrogen source. Separate the female and male ports of the leak-proof interface 10. The female and male ports are referred to as the female port and female port, respectively.

[0052] Step 3: Connect sample collection port 8 to the cyanopyridine pipeline in the device. Manually open the female port of the leak-proof interface 10 and control the sample injection structure 7 to pump cyanopyridine into the pipeline for rinsing. Collect the rinsed cyanopyridine back into the waste liquid tank for centralized disposal. After rinsing, control the sample injection structure 7 to stop pumping, close the female port, and wipe the interface clean.

[0053] Step 4: Connect the female and female ports of the leak-proof interface 10, and control the injection structure 7 to pump in 0.77g of cyanopyridine, which translates to approximately 0.85ml of liquid. This process is completed collaboratively by the injection structure 7 and the gravimetric testing device 5. When the gravimetric testing device 5 detects that the sample mass is close to the set value, it controls the injection structure 7 to slow down the injection speed, ultimately ensuring precise material addition. After material addition is complete, separate the female and female ports of the leak-proof interface 10, and disconnect the connection between the collection port 8 and the cyanopyridine tubing.

[0054] Step 5: Remove the sample inlet 76, sample inlet 78, and sample outlet 710 from the sample inlet structure 7, and replace them together with a new clean sampling and sample inlet pipeline, along with the sampling port 8, the female port of the leak-proof interface 10, and the pipeline. Then, perform nitrogen purging as described in Step 2.

[0055] Step 6: Using the central controller of the control structure 9, the temperature of the test container 2 and the reference container 3 is reduced to 0°C by the temperature control and calorimetry device 1.

[0056] Step 7: Connect the new sample collection port 8 to the ethyl magnesium chloride pipeline in the device. Manually open the female port of the leak-proof interface 10, and control the sample injection structure 7 to pump ethyl magnesium chloride into the pipeline for rinsing. Collect the rinsed ethyl magnesium chloride back into the waste liquid tank for centralized disposal. After rinsing, control the sample injection structure 7 to stop pumping, close the female port, and wipe the interface clean.

[0057] Step 8: Connect the female and male ports of the leak-proof interface 10, and control the injection structure 7 to pump in 0.64g of ethyl magnesium chloride solution, which translates to approximately 0.71ml of liquid. This process is completed collaboratively by the injection structure 7 and the weight testing device 5. When the weight testing device 5 detects that the sample mass is close to the set value, it controls the injection structure 7 to slow down the injection speed, ultimately ensuring precise material addition.

[0058] Step 9: Through the central control system of control structure 9, the temperature of test container 2 and test container 3 is gradually raised to 20°C using temperature control and calorimetry device 1, with a heating time of 6 hours. The heat flow of test container 2 and reference container 3 is obtained by temperature sensors in temperature control and calorimetry device 1.

[0059] Step 10: The reaction heat is calculated using the software built into the central control system of control structure 9. The reaction heat flux is obtained by subtracting the heat flux of the reference container from the heat flux of the test container 2. The calculation formula is as follows: ΔW = dQs / dt - dQr / dt = dH / dt dQs / dt: Heat delivered to the test container per unit time; dQr / dt: Heat supplied to the reference container per unit time; dH / dt: Enthalpy change rate.

[0060] Integrating the heat flux yields a reaction heat of 27 J. Further calculations reveal the enthalpy of the imine preparation reaction to be approximately -7 kJ / mol (based on ethyl magnesium chloride).

[0061] Example 5 Chloropyridine is prepared by reacting chloropyridinone with phosgene.

[0062] Step 1: Assemble and connect all components of the calorimeter according to the overall schematic diagram of this chemical reaction calorimeter. Place the clean glass test container 2 and reference container 3 on the weight testing device 5 in the temperature control and calorimeter device 1. Add the stir bar 4 to the test container 1. Connect the pressure sensor 6 and the female port of the leak-proof interface 10 to the top of the test container 2. Connect the female port of the leak-proof interface to the outlet of the sample inlet structure 7. Connect the inlet of the sample inlet structure 7 to the sample collection port 8. Connect the calorimeter to the central control system 9 via a data cable.

[0063] Step 2: Connect sample collection port 8 to the nitrogen source. Control the sample injection structure 7 to continuously pump nitrogen into the test device along the pipeline, purging air from the pipeline and test container 2. The nitrogen purging time is 10 minutes. After purging, control the sample injection structure 7 to stop pumping and disconnect the sample collection port 8 from the nitrogen source. Separate the male and female ports of the leak-proof interface 10.

[0064] Step 3: Connect sample collection port 8 to the 30% chloropyridinone solution pipeline in the device. Manually open the female port of the leak-proof interface 10, and control the sample injection structure 7 to pump the chloropyridinone solution into the pipeline for rinsing. Collect the rinsed chloropyridinone solution back into the waste liquid tank for centralized disposal. After rinsing, control the sample injection structure 7 to stop pumping, close the female port, and wipe the interface clean.

[0065] Step 4: Connect the female and female ports of the leak-proof interface 10, and control the injection structure 7 to pump in 1.2g of chloropyridinone solution, which translates to approximately 1.0ml of liquid. This process is completed collaboratively by the injection structure 7 and the gravimetric testing device 5. When the gravimetric testing device 5 detects that the sample mass is close to the set value, it controls the injection structure 7 to slow down the injection speed, ultimately ensuring precise material addition. After material addition is complete, separate the female and female ports of the leak-proof interface 10 and disconnect the connection between the collection port 8 and the chloropyridinone solution tubing.

[0066] Step 5: Remove the sample inlet 76, sample inlet 78, and sample outlet 710 from the sample inlet structure 7, and replace them together with a new clean sampling and sample inlet pipeline, along with the female port of the sampling port 8 and the leak-proof interface 10. Then, purge with nitrogen as described in Step 2.

[0067] Step 6: Using the central controller 9 and the temperature control and calorimetry device 1, the temperature of the test container 2 and the reference container 3 is controlled to approximately 20°C.

[0068] Step 7: Connect the new sample collection port 8 to the phosgene solution pipeline in the device. Manually open the female port of the leak-proof interface 10, and control the sample injection structure 7 to pump the phosgene solution into the pipeline for rinsing. Collect the rinsed phosgene solution back into the dedicated waste liquid tank for centralized disposal. After rinsing, control the sample injection structure 7 to stop pumping, close the female port, and wipe the interface clean.

[0069] Step 8: Connect the female and male ports of the leak-proof interface 10, and control the injection structure 7 to pump in 0.30g of phosgene solution, which translates to approximately 0.25ml of liquid volume. This process is completed collaboratively by the injection structure 7 and the weight testing device 5. When the weight testing device 5 detects that the sample mass is close to the set value, it controls the injection structure 7 to slow down the injection speed, ultimately ensuring precise material addition.

[0070] Step 9: Through the central control system of control structure 9, the temperature of test container 2 and test container 3 is gradually raised to 80°C using temperature control and calorimetry device 1. The heating time is 4 hours, and the temperature is kept constant for 4 hours. The heat flow of test container 2 and reference container 3 is obtained by temperature sensor in temperature control and calorimetry device 1.

[0071] Step 10: The reaction heat is calculated using the software built into the central control system of control structure 9. The heat flow of the reaction is obtained by subtracting the heat flow of the reference container from the heat flow of the test container 2. Integrating the heat flow yields the reaction heat of 256 J. Further calculations show that the enthalpy of the monochloropyridinone preparation reaction is approximately -306 kJ / mol (based on chloropyridinone).

[0072] Example 6 p-Tolyl magnesium chloride (Grignard reagent) is prepared by reacting p-methyliodobenzene with ethyl magnesium chloride (Grignard reagent).

[0073] Step 1: Assemble and connect all components of the calorimeter according to the overall schematic diagram of this chemical reaction calorimeter. Place the clean glass test container 2 and reference container 3 on the weight testing device 5 in the temperature control and calorimeter device 1. Add the stir bar 4 to the test container 1. Connect the pressure sensor 6 and the female port of the leak-proof interface 10 to the top of the test container 2. Connect the female port of the leak-proof interface to the outlet of the sample inlet structure 7. Connect the inlet of the sample inlet structure 7 to the sample collection port 8. Connect the calorimeter to the central control system 9 via a data cable.

[0074] Step 2: Connect sample collection port 8 to the nitrogen source. Control the sample injection structure 7 to continuously pump nitrogen into the test device along the pipeline, purging air from the pipeline and test container 2. The nitrogen purging time is 10 minutes. After purging, control the sample injection structure 7 to stop pumping and disconnect the sample collection port 8 from the nitrogen source. Separate the male and female ports of the leak-proof interface 10.

[0075] Step 3: Connect sample collection port 8 to the p-methyliodobenzene pipeline in the device. Manually open the female port of the leak-proof interface 10 and control the sample injection structure 7 to pump p-methyliodobenzene into the pipeline for rinsing. Collect the rinsed p-methyliodobenzene into the waste liquid tank for centralized disposal. After rinsing, control the sample injection structure 7 to stop pumping, close the female port, and wipe the interface clean.

[0076] Step 4: Connect the female and female ports of the leak-proof interface 10, and control the injection structure 7 to pump in 1.22g of p-methyliodobenzene solution, which translates to approximately 1.35ml of liquid. This process is completed collaboratively by the injection structure 7 and the weight testing device 5. When the weight testing device 5 detects that the sample mass is close to the set value, it controls the injection structure 7 to slow down the injection speed, ultimately ensuring precise material addition. After material addition is complete, separate the female and female ports of the leak-proof interface 10 and disconnect the connection between the collection port 8 and the p-methyliodobenzene tubing.

[0077] Step 5: Remove the sample inlet 76, sample inlet 78, and sample outlet 710 from the sample inlet structure 7, and replace them together with a new clean sampling and sample inlet pipeline, along with the female port of the sampling port 8 and the leak-proof interface 10. Then, purge with nitrogen as described in Step 2.

[0078] Step 6: Using the central controller 9 and the temperature control and calorimetry device 1, the temperature of the test container 2 and the reference container 3 is reduced to 0°C.

[0079] Step 7: Connect the new sample collection port 8 to the isopropyl magnesium chloride pipeline in the device. Manually open the female port of the leak-proof interface 10, and control the sample injection structure 7 to pump the isopropyl magnesium chloride into the pipeline for rinsing. Collect the rinsed isopropyl magnesium chloride back into the waste liquid tank for centralized disposal. After rinsing, control the sample injection structure 7 to stop pumping, close the female port, and wipe the interface clean.

[0080] Step 8: Connect the female and male ports of the leak-proof interface 10, and control the injection structure 7 to pump in 0.28g of isopropyl magnesium chloride solution, which translates to approximately 0.31ml of liquid. This process is completed collaboratively by the injection structure 7 and the weight testing device 5. When the weight testing device 5 detects that the sample mass is close to the set value, it controls the injection structure 7 to slow down the injection speed, ultimately ensuring precise material addition.

[0081] Step 9: Through the central control system of control structure 9, the temperature of test container 2 and test container 3 is gradually raised to 15°C using temperature control and calorimetry device 1. The heating time is 2 hours, and the temperature is kept constant for 2 hours. The heat flow of test container 2 and reference container 3 is obtained by temperature sensor in temperature control and calorimetry device 1.

[0082] Step 10: The reaction heat is calculated using the software built into the central control system of control structure 9. The heat flow of the reaction is obtained by subtracting the heat flow of the reference container from the heat flow of the test container 2. Integrating the heat flow yields the reaction heat of 28 J. Further calculations show that the enthalpy of the reaction for the preparation of p-tolyl magnesium chloride is approximately -116 kJ / mol (based on ethyl magnesium chloride).

[0083] Example 7 The reaction of cyanopyridine with ethyl magnesium chloride (Grignard reagent) to prepare an imine compound (Grignard reagent) was carried out without nitrogen purging of the pipelines and equipment.

[0084] Step 1: Assemble and connect the various components of the equipment according to the overall schematic diagram of this chemical reaction calorimeter.

[0085] Step 2: Connect the sample collection port to the cyanopyridine tubing in the device, discharge a small amount of cyanopyridine for rinsing, recover the rinsing solution and clean the interface.

[0086] Step 3: Connect the tubing to the testing equipment and pump in 0.77g (approximately 0.85ml) of cyanopyridine. Disconnect the injection tubing after sampling is complete.

[0087] Step 4: Replace with a new, clean set of sampling and injection tubing.

[0088] Step 5: Adjust the test solution to 0°C.

[0089] Step 6: Connect the new sample collection port to the ethyl magnesium chloride tubing in the device, drain a small amount of ethyl magnesium chloride for rinsing, recover the rinsing solution and clean the interface.

[0090] Step 7: Connect the tubing to the testing equipment and pump in 0.64g of ethyl magnesium chloride (approximately 0.71ml). Disconnect the sample inlet tubing after sampling is complete.

[0091] Step 8: Control the temperature of the test system to gradually increase to 20°C over 6 hours, and obtain the heat flow of the test sample through the temperature sensor.

[0092] Step 9: Calculate the heat of reaction.

[0093] Integrating the heat flux yields a reaction heat of 9 J. Further calculations reveal the enthalpy of the imine preparation reaction to be approximately -2 kJ / mol (based on ethyl magnesium chloride).

[0094] Example 8 The preparation of monochloropyridine by reacting chloropyridinone with phosgene was carried out without nitrogen purging of the pipelines and equipment.

[0095] Step 1: Assemble and connect the various components of the equipment according to the overall schematic diagram of this chemical reaction calorimeter.

[0096] Step 2: Connect the sample collection port to the chloropyridinone tubing in the device, discharge a small amount of chloropyridinone for rinsing, recover the rinsing solution and clean the interface.

[0097] Step 3: Connect the tubing to the testing equipment and pump in 1.2g (approximately 1.0ml) of chloropyridinone. Disconnect the injection tubing after sampling is complete.

[0098] Step 4: Replace with a new, clean set of sampling and injection tubing.

[0099] Step 5: Adjust the test solution to 20°C.

[0100] Step 6: Connect the new sample collection port to the phosgene solution pipeline in the device, discharge a small amount of phosgene solution for rinsing, recover the rinsing solution and clean the interface.

[0101] Step 7: Connect the tubing to the testing equipment and pump in 0.30g (approximately 0.25ml) of phosgene solution. Disconnect the sample inlet tubing after sampling is complete.

[0102] Step 8: Control the temperature of the test system to gradually increase to 80℃ over 4 hours, maintain the temperature for 4 hours, and obtain the heat flow of the test sample through the temperature sensor.

[0103] Step 9: Calculate the heat of reaction.

[0104] Integrating the heat flux yields a reaction heat of 201 J. Further calculations reveal the enthalpy of the chloropyridinone preparation reaction to be approximately -240 kJ / mol (based on chloropyridinone).

[0105] Example 9 p-Tolyl magnesium chloride (Grignard reagent) was prepared by reacting p-methyliodobenzene with ethyl magnesium chloride (Grignard reagent), without purging the pipelines and equipment with nitrogen.

[0106] Step 1: Assemble and connect the various components of the equipment according to the overall schematic diagram of this chemical reaction calorimeter.

[0107] Step 2: Connect the sample collection port to the methyl iodobenzene tubing in the device, discharge a small amount of methyl iodobenzene for rinsing, recover the rinsing solution and clean the interface.

[0108] Step 3: Connect the tubing to the testing equipment and pump in 1.22g of methyliodobenzene (approximately 1.35ml). Disconnect the sample inlet tubing after sampling is complete.

[0109] Step 4: Replace with a new, clean set of sampling and injection tubing.

[0110] Step 5: Adjust the test solution to 0°C.

[0111] Step 6: Connect the new sample collection port to the ethyl magnesium chloride solution pipeline in the device, drain a small amount of ethyl magnesium chloride solution to rinse, recover the rinsing solution and clean the interface.

[0112] Step 7: Connect the tubing to the testing equipment and pump in 0.28g (approximately 0.31ml) of ethyl magnesium chloride solution. Disconnect the sample inlet tubing after sampling is complete.

[0113] Step 8: Control the temperature of the test system to gradually increase to 15°C within 2 hours, maintain the temperature for 2 hours, and obtain the heat flow of the test sample through the temperature sensor.

[0114] Step 9: Calculate the heat of reaction.

[0115] Integrating the heat flux yields a reaction heat of 14 J. Further calculations reveal the reaction enthalpy for the preparation of toluene-magnesium chloride to be approximately -56 kJ / mol (based on ethyl magnesium chloride).

[0116] Example 10 The reaction of cyanopyridine with ethyl magnesium chloride (Grignard reagent) to prepare an imine compound (Grignard reagent) was carried out without changing the tubing.

[0117] Step 1: Assemble and connect the various components of the equipment according to the overall schematic diagram of this chemical reaction calorimeter.

[0118] Step 2: Connect the sample collection port to the nitrogen gas source and rewash the pipeline and equipment with nitrogen.

[0119] Step 3: Connect the sample collection port to the cyanopyridine tubing in the device, discharge a small amount of cyanopyridine for rinsing, recover the rinsing solution and clean the interface.

[0120] Step 4: Connect the tubing to the testing equipment and pump in 0.77g (approximately 0.85ml) of cyanopyridine. Disconnect the sample inlet tubing after sampling is complete.

[0121] Step 5: Adjust the test solution to 0°C.

[0122] Step 6: Connect the sample collection port to the ethyl magnesium chloride pipeline in the device, discharge a small amount of ethyl magnesium chloride for rinsing, recover the rinsing solution and clean the interface.

[0123] Step 7: Connect the tubing to the testing equipment and pump in 0.64g of ethyl magnesium chloride (approximately 0.71ml). Disconnect the sample inlet tubing after sampling is complete.

[0124] Step 8: Control the temperature of the test system to gradually increase to 20°C over 6 hours, and obtain the heat flow of the test sample through the temperature sensor.

[0125] Step 9: Calculate the heat of reaction.

[0126] Integrating the heat flux yields a reaction heat of 15 J. Further calculations reveal the enthalpy of the imine preparation reaction to be approximately -3 kJ / mol (based on ethyl magnesium chloride).

[0127] Example 11 Chloropyridone was reacted with phosgene to prepare chloropyridine without changing the pipeline.

[0128] Step 1: Assemble and connect the various components of the equipment according to the overall schematic diagram of this chemical reaction calorimeter.

[0129] Step 2: Connect the sample collection port to the nitrogen gas source and rewash the pipeline and equipment with nitrogen.

[0130] Step 3: Connect the sample collection port to the chloropyridinone tubing in the device, discharge a small amount of chloropyridinone for rinsing, recover the rinsing solution and clean the interface.

[0131] Step 4: Connect the tubing to the testing equipment and pump in 1.2g (approximately 1.0ml) of chloropyridinone. Disconnect the injection tubing after sampling is complete.

[0132] Step 5: Adjust the test solution to 20°C.

[0133] Step 6: Connect the sample collection port to the phosgene solution pipeline in the device, discharge a small amount of phosgene solution for rinsing, recover the rinsing solution and clean the interface.

[0134] Step 7: Connect the tubing to the testing equipment and pump in 0.30g (approximately 0.25ml) of phosgene solution. Disconnect the sample inlet tubing after sampling is complete.

[0135] Step 8: Control the temperature of the test system to gradually increase to 80℃ over 4 hours, maintain the temperature for 4 hours, and obtain the heat flow of the test sample through the temperature sensor.

[0136] Step 9: Calculate the heat of reaction.

[0137] Integrating the heat flux yields the heat of reaction, which is 121 J. Further calculations reveal the enthalpy of the reaction for the preparation of chloropyridinone to be approximately -145 kJ / mol (based on chloropyridinone).

[0138] Example 12 p-Tolyl magnesium chloride (Grignard reagent) was prepared by reacting p-methyliodobenzene with ethyl magnesium chloride (Grignard reagent), without purging the pipelines and equipment with nitrogen.

[0139] Step 1: Assemble and connect the various components of the equipment according to the overall schematic diagram of this chemical reaction calorimeter.

[0140] Step 2: Connect the sample collection port to the nitrogen gas source and rewash the pipeline and equipment with nitrogen.

[0141] Step 3: Connect the sample collection port to the methyl iodobenzene tubing in the device, drain a small amount of methyl iodobenzene for rinsing, and do not replace the tubing.

[0142] Step 4: Connect the tubing to the testing equipment and pump in 1.22g of methyliodobenzene (approximately 1.35ml). Disconnect the injection tubing after sampling is complete.

[0143] Step 5: Adjust the test solution to 0°C.

[0144] Step 6: Connect the sample collection port to the ethyl magnesium chloride solution pipeline in the device, drain a small amount of ethyl magnesium chloride solution to rinse, recover the rinsing solution and clean the interface.

[0145] Step 7: Connect the tubing to the testing equipment and pump in 0.28g (approximately 0.31ml) of ethyl magnesium chloride solution. Disconnect the sample inlet tubing after sampling is complete.

[0146] Step 8: Control the temperature of the test system to gradually increase to 15°C within 2 hours, maintain the temperature for 2 hours, and obtain the heat flow of the test sample through the temperature sensor.

[0147] Step 9: Calculate the heat of reaction.

[0148] Integrating the heat flux yields a reaction heat of 9 J. Further calculations reveal the reaction enthalpy for the preparation of toluene-magnesium chloride to be approximately -36 kJ / mol (based on ethyl magnesium chloride).

[0149] Data Comparison Table 1. Comparison of synthesis reactions of imine compounds (Grignard reagents) .

[0150] Table 2 Comparison of Monochloropyridine Synthesis Reactions .

[0151] Table 3 Comparison of Synthesis Reactions for Tolyl Magnesium Chloride (Grignard Reagent) .

[0152] The above embodiments are merely illustrative of the inventive concept and features of the present invention, intended to enable those skilled in the art to understand the content of the present invention and implement it accordingly, and should not be construed as limiting the scope of protection of the present invention. All equivalent changes or modifications made based on the essence of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A portable device for measuring the heat of chemical reaction, characterized in that: The device includes a housing, a temperature control and calorimetry device, a weight testing device, a sample introduction structure, a control structure, and a leak-proof interface. The temperature control and calorimetry device includes a temperature sensor, a test container, and a reference container. The test container and the reference container are arranged parallel to each other within the housing. The temperature sensor measures the temperature changes within the test container and the reference container and sends the temperature change data to the control structure. The weight testing device is located below the test container and is used to monitor and record the weight changes of the material within the test container and send the weight change data to the control structure. The sample introduction structure is connected to the test container through the leak-proof interface and provides a sample to the temperature control and calorimetry device. A pressure sensor is installed on the outside of the test container. The control structure also includes a reaction heat calculation program.

2. The portable device for measuring the heat of chemical reaction according to claim 1, characterized in that: The temperature control and calorimetry device also includes a stir bar, which is disposed at the bottom of the test container and the reference container.

3. The portable device for measuring the heat of chemical reaction according to claim 1, characterized in that: The sample injection structure includes a sample injection motor, a sample injection chamber, a sample inlet, a sample outlet, a piston, and a push rod. A push rod hole is provided at the bottom of the sample injection chamber. The piston is disposed in the sample injection chamber. One end of the push rod is connected to the piston, and the other end passes through the push rod hole and is connected to the output end of the sample injection motor. The sample injection motor drives the piston to reciprocate within the sample injection chamber. The sample inlet and sample outlet are disposed on the chamber wall above the piston. A sample collection port is provided on the outside of the sample inlet, and the sample outlet is connected to the leak-proof interface.

4. The portable device for measuring the heat of chemical reaction according to claim 3, characterized in that: The sample injection structure also includes two one-way valves, which are respectively located at the sample inlet and the sample outlet. Under the action of the piston and the one-way valves, when the piston moves downward, the sample enters the sample injection chamber through the sample inlet. When the piston moves upward, the sample leaves the sample injection chamber through the sample outlet.

5. The portable device for measuring the heat of chemical reaction according to claim 4, characterized in that: The leak-proof interface includes a female interface and a female interface. The female interface is fitted inside the female interface. The female interface is connected to the sample outlet, and the female interface is connected to the test container.

6. The portable device for measuring the heat of chemical reaction according to claim 5, characterized in that: The female port includes a female port shell, a female port pipeline, an annular cavity, a female port isolator, a female port spring, and a female port fixing buckle. The female port pipeline is located inside the female port shell and has a first sample port. The top end of the female port pipeline is closed, and the bottom end is connected to the sample outlet. The annular cavity is formed between the female port shell and the female port pipeline. The female port isolator is sleeved on the top of the female port pipeline and moves up and down within the annular cavity. The female port spring is located at the bottom of the female port isolator. The female port fixing buckle is located inside the female port shell to limit the position of the female port isolator.

7. The portable device for measuring the heat of chemical reaction according to claim 6, characterized in that: The interface sub-port includes a sub-port outer shell, a sub-port inner tube, a sub-port outer tube, a sub-port isolator, a sub-port spring, and a sub-port pipeline support. The sub-port outer shell is inserted into the annular cavity. The sub-port inner tube and the sub-port outer tube are located inside the sub-port outer shell. The sub-port inner tube has a sub-port hole. The sub-port inner tube communicates with the outside through its top and is closed at its bottom. The sub-port outer tube is located on the other side of the sub-port hole and is connected to the test container. The sub-port isolator is slidably sleeved on the inside of the sub-port inner tube to open and close the sub-port hole. The sub-port spring is located between the sub-port isolator and the bottom wall of the sub-port inner tube. The sub-port pipeline support is located between the sub-port inner tube and the sub-port outer tube to fix the sub-port inner tube.

8. The portable device for measuring the heat of chemical reaction according to claim 1, characterized in that: The control structure also includes a differential thermal amplifier, a power compensator, a data acquisition unit, and a thermocouple cold junction compensator. When the sample reacts exothermically in the test container, the temperature of the test container is higher than the temperature of the reference container. The thermocouple in the temperature control and calorimetry device will generate a temperature difference potential, which is amplified by the differential thermal amplifier and sent to the power compensator. The control structure automatically reduces the temperature of the test container based on the data feedback from the data acquisition unit, so that the temperature difference between the test container and the reference container approaches zero. The thermocouple cold junction compensation device is used to eliminate the error caused by the temperature difference between the thermocouple and the test container.

9. A test method for a portable device for measuring the heat of chemical reaction, characterized in that, Includes the following steps: Step 1: Assemble the portable device for measuring the heat of chemical reaction according to any one of claims 1-8, connect the temperature control and calorimetry device to the control structure using a data cable, connect the sample injection structure to the nitrogen source, and purge the pipeline with nitrogen. Add a certain amount of reference material to the reference pipeline in advance. Step 2: Connect the injection device to the sample one pipeline, control the injection device to pump the sample one into the pipeline for rinsing, after rinsing is completed, control the injection device to stop pumping, close the female port and wipe the interface dry; Step 3: Connect the injection structure and the test container, control the injection structure to pump in sample one, when the weight test structure detects that sample one is close to the limit value, it sends a signal to the control structure, the control structure controls the injection structure to slow down the injection speed, and accurately add the material. After the material is added, disconnect the injection structure from the test container. Step 4: Replace the injection structure and the tubing connected to the test container, reconnect them, and connect the newly connected injection structure to the nitrogen source, and purge the tubing with nitrogen. Step 5: Adjust the temperature control and calorimeter to the initial temperature using the control structure; Step 6: Connect the injection structure from Step 4 to the sample two pipeline, control the injection structure to pump the sample two into the pipeline for rinsing, after rinsing is completed, control the injection structure to stop pumping, close the female port and wipe the interface dry. Step 7: Connect the injection structure and the test container, control the injection structure to pump in sample two. When the weight test structure detects that sample two is close to the limit value, it sends a signal to the control structure. The control structure controls the injection structure to slow down the injection speed and accurately add the material. After the material is added, disconnect the injection structure from the test container. Step 8: Adjust the temperature in the temperature control and calorimeter to the reaction temperature using the control structure, control the heating time, and obtain the heat flow in the test container and reference container respectively through temperature sensors. Step 9: Perform reaction heat calculation using the reaction heat calculation program of the control structure to obtain the heat flow of the reaction.

10. The test method of the portable device for measuring the heat of chemical reaction according to claim 9, characterized in that, In step 9, the heat flux of the reaction is obtained by subtracting the heat flux of the reference container from the heat flux of the test container, and the calculation formula is as follows: ΔW = dQs / dt - dQr / dt = dH / dt, where dQs / dt represents the heat supplied to the test container per unit time, dQr / dt represents the heat supplied to the reference container per unit time, and dH / dt represents the rate of change of enthalpy.

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