Adiabatic accelerating calorimeter based on electromagnetic heating technology

Abstract

The present invention provides an adiabatic accelerating calorimeter based on electromagnetic heating technology, the structure of which comprises an adiabatic accelerating calorimeter furnace body (1), an adiabatic accelerating calorimeter furnace cover (2), a sample pool (3), a temperature control system (4), an adiabatic accelerating calorimeter furnace body insulation cotton (5), and a furnace body electromagnetic induction coil placement area (6); the sample pool (3) is located inside the adiabatic accelerating calorimeter furnace body (1), the adiabatic accelerating calorimeter furnace cover (2) is located at the furnace body opening of the adiabatic accelerating calorimeter furnace body (1), the adiabatic accelerating calorimeter furnace body insulation cotton (5) is wrapped around the adiabatic accelerating calorimeter furnace body (1), and the furnace body electromagnetic induction coil placement area (6) is located outside the adiabatic accelerating calorimeter furnace body insulation cotton (5); the temperature control system (4) comprises a furnace body electromagnetic induction coil (42) and a sample pool electromagnetic induction coil (44).

Description

Technical Field

[0001] The invention relates to an adiabatic accelerating calorimeter based on electromagnetic heating technology, and belongs to the field of accelerating calorimetry technology and instruments for chemical process safety. Background Art

[0002] Adiabatic accelerating rate calorimeter is an important tool for analyzing chemical reactions and evaluating the thermal hazards of hazardous chemicals. It plays an important role in reducing accidents caused by thermal runaway.

[0003] Nowadays, adiabatic accelerating calorimeters on the market generally have two heating methods at the same time: one is to heat the furnace body with a heating rod so that the temperature of the furnace body tracks the temperature change of the sample pool and keeps the two consistent as much as possible; the other sample heater is to install a metal heating wire on the bottom of the furnace body to heat the sample pool through thermal radiation; although the traditional resistance wire heating method has the advantages of low price and simple installation, the heat loss is particularly large, and most of the heat will be dissipated into the air during heating, resulting in a waste of electric energy, and the service life is also short, and the thermal hysteresis is relatively large, often failing to reach the temperature rise rate during the thermal runaway reaction of the sample, which is not conducive to precise temperature control, and the adiabatic accelerating calorimeter has very high requirements for temperature accuracy; high-frequency electromagnetic heating technology is the cutting-edge technology in the field of electric heating, which has high heating efficiency, fast speed, green environmental protection and low consumption for metal materials; the heat conversion rate of electromagnetic heating is quite high, up to 95%, and the startup is also very fast, and the preheating time is reduced by more than 60% compared with resistance wire heating.

[0004] The adiabatic accelerating calorimeter needs to maintain an insulated environment inside the furnace, that is, the sample temperature is equal to the temperature of the furnace. The above is the first-level temperature tracking, and the second-level temperature tracking is the sample temperature being tracked by the sample pool wall temperature. The electromagnetic heating method can quickly heat up the furnace and sample pool wall temperatures, and track the sample temperature when the chemical reaction rate is high. Summary of the invention

[0005] The present invention provides an adiabatic accelerating calorimeter based on electromagnetic heating technology, which aims to overcome the problems of excessive heat loss and slow heating speed caused by traditional resistance wire heating.

[0006] The technical solution of the present invention is: an adiabatic accelerating calorimeter based on electromagnetic heating technology, whose structure includes an adiabatic accelerating calorimeter furnace body 1, an adiabatic accelerating calorimeter furnace cover 2, a sample pool 3, a temperature control system 4, an adiabatic accelerating calorimeter furnace body insulation cotton 5, and a furnace body electromagnetic induction coil placement area 6; the sample pool 3 is located inside the adiabatic accelerating calorimeter furnace body 1, the adiabatic accelerating calorimeter furnace cover 2 is located at the furnace body mouth of the adiabatic accelerating calorimeter furnace body 1, the adiabatic accelerating calorimeter furnace body insulation cotton 5 is wrapped around the adiabatic accelerating calorimeter furnace body 1, and the furnace body electromagnetic induction coil placement area 6 is located on the periphery of the adiabatic accelerating calorimeter furnace body insulation cotton 5; the temperature control system 4 includes a furnace body electromagnetic induction coil 42 and a sample pool electromagnetic induction coil 44, the furnace body electromagnetic induction coil 42 is installed in the furnace body electromagnetic induction coil placement area 6, and the sample pool electromagnetic induction coil 44 is installed on the periphery of the sample pool 3.

[0007] Beneficial effects of the present invention:

[0008] 1. The adiabatic accelerating calorimeter using electromagnetic heating method, using a high-frequency heating device and electromagnetic heating method, can not only heat up the adiabatic accelerating calorimeter furnace, sample pool and the sample to be tested in the sample pool in the initial stage, but also heat the adiabatic accelerating calorimeter furnace body and the sample pool wall when the sample to be tested reaches the reaction temperature and starts to undergo a thermal runaway reaction, so that the temperature of the adiabatic accelerating calorimeter furnace body is equal to the temperature of the sample pool wall and the temperature of the sample pool wall is equal to the real-time temperature of the sample; it solves the problem of excessive heat loss and slow heating speed in the traditional heating process, which causes hysteresis when the adiabatic accelerating calorimeter performs temperature tracking in the thermal runaway stage of chemicals;

[0009] 2. The present invention adopts high-frequency electromagnetic heating, using high-frequency current to pass through the electromagnetic induction coil to generate magnetic field force. When the magnetic force in the magnetic field passes through the cylindrical sample pool wall, countless small eddy currents will be generated inside, causing it to heat up at high speed, greatly increasing the temperature rise rate of the sample pool wall, speeding up the secondary temperature tracking speed, reducing the measurement error caused by temperature tracking lag, and facilitating more accurate thermodynamic calculations;

[0010] 3. The electromagnetic induction coil used in the present invention will generate a high-speed changing alternating magnetic field when a fast-changing high-frequency high-voltage current flows through it, which can convert the 220V alternating current into a high-frequency alternating current of 20KHZ-40KHZ. The adiabatic accelerating calorimeter furnace and the cylindrical sample cell are electromagnetically induced in the magnetic field to generate eddy currents. When the induced current flows in the conductor, the thermal effect of the conductor converts the electrical energy into the internal energy of the conductor, thereby heating the conductor.

[0011] 4. The present invention ensures that the test sample is in an adiabatic state when the reaction occurs, which is conducive to obtaining more accurate thermodynamic parameters, making the thermal hazard assessment of chemicals closer to the actual situation, overcoming the problems of excessive heat loss and slow heating speed caused by traditional resistance wire heating methods, and is of great significance for implementing more accurate safety risk assessments and chemical safety evaluations. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Attached Figure 1 This is a schematic structural diagram of an adiabatic accelerating calorimeter using electromagnetic heating proposed by the present invention.

[0013] Attached Figure 2 It is a cross-sectional view of the cylindrical sample cell in Example 1.

[0014] Attached Figure 3 This is the connection diagram of the temperature control system.

[0015] Attached Figure 4 It is a cross-sectional view of the cylindrical sample cell in Example 2.

[0016] Attached Figure 5 Schematic diagram of the sample cell and its heating element.

[0017] In the accompanying drawings, 1 is an adiabatic accelerating calorimeter furnace body, 2 is an adiabatic accelerating calorimeter furnace cover, 3 is a cylindrical sample pool, 31 is a feeding channel, 32 is a reaction zone, 33 is a sample to be tested, 4 is a temperature control system, 41 is a 220V AC power supply, 42 is a furnace body electromagnetic induction coil, 43 is a temperature measuring module, 44 is a sample pool electromagnetic induction coil, 45 is an electromagnetic protection net, 46 is an electromagnetic heating controller, 47 is a temperature measuring thermocouple, 471 is a furnace cover temperature measuring thermocouple, 472 is a furnace side temperature measuring thermocouple, 473 is a furnace bottom temperature measuring thermocouple, 474 is a sample pool side wall temperature measuring thermocouple, 475 is a sample temperature measuring thermocouple, 476 is a sample pool bottom temperature measuring thermocouple, 48 is a switch, 49 is a computer, 5 is adiabatic accelerating calorimeter furnace body insulation cotton, 6 is a furnace body electromagnetic induction coil placement area, and 7 is a sample pool insulation cotton. DETAILED DESCRIPTION

[0018] The invention discloses an adiabatic accelerating calorimeter based on electromagnetic heating technology, which comprises an adiabatic accelerating calorimeter furnace body 1, an adiabatic accelerating calorimeter furnace cover 2, a sample pool 3, a temperature control system 4, an adiabatic accelerating calorimeter furnace body insulation cotton 5, and a furnace body electromagnetic induction coil placement area 6; the sample pool 3 is located inside the adiabatic accelerating calorimeter furnace body 1, the adiabatic accelerating calorimeter furnace cover 2 is located at the furnace body mouth of the adiabatic accelerating calorimeter furnace body 1, the adiabatic accelerating calorimeter furnace body insulation cotton 5 is wrapped around the adiabatic accelerating calorimeter furnace body 1, and the furnace body electromagnetic induction coil placement area 6 is located on the periphery of the adiabatic accelerating calorimeter furnace body insulation cotton 5; the temperature control system 4 comprises a furnace body electromagnetic induction coil 42 and a sample pool electromagnetic induction coil 44, the furnace body electromagnetic induction coil 42 is installed in the furnace body electromagnetic induction coil placement area 6, and the sample pool electromagnetic induction coil 44 is installed on the periphery of the sample pool 3.

[0019] The sample pool 3 is preferably a cylindrical sample pool.

[0020] The adiabatic accelerating calorimeter furnace body 1 has a cavity inside, the upper end of the cavity is the furnace body opening, the sample pool 3 is located in the cavity inside the adiabatic accelerating calorimeter furnace body 1, and the upper end of the sample pool 3 is connected to the adiabatic accelerating calorimeter furnace cover 2 at the furnace body opening through a bolt sleeve.

[0021] The temperature control system 4 also includes an AC power supply 41, a temperature measuring module 43, an electromagnetic protection net 45, an electromagnetic heating controller 46, a temperature measuring thermocouple 47, a switch 48, and a computer 49; the signal input and output ends of the computer 49 are correspondingly connected to the signal output and input ends of the switch 48, the signal input end of the switch 48 is connected to the signal output end of the temperature measuring module 43, the signal input end of the temperature measuring module 43 is connected to the signal output end of the temperature measuring thermocouple 47, and the signal output end of the computer 49 is connected to the first signal input end of the electromagnetic heating controller 46; the computer 49 can be used to control heating and display and analyze data.

[0022] The AC power source 41 is preferably a 220V AC power source.

[0023] The power port of the electromagnetic heating controller 46 is connected to the AC power supply 41 , the first signal input / output port of the electromagnetic heating controller 46 is connected to the furnace electromagnetic induction coil 42 , and the second signal input / output port of the electromagnetic heating controller 46 is connected to the sample pool electromagnetic induction coil 44 .

[0024] The electromagnetic heating controller 46 includes an IGBT (Insulated Gate Bipolar Transistor) module, and the electromagnetic heating controller 46 can adjust the power through the IGBT module.

[0025] The temperature measuring thermocouple 47 is connected to the temperature measuring module 43. The temperature measuring module 43 converts the current signal of the temperature measuring thermocouple 47 into a digital signal, and outputs it to the computer 49 through the switch 48 using the Modbus TCP communication protocol, and reads the data through the computer 49; the computer 49 controls the output pulse signal to the IGBT module of the electromagnetic heating controller 46 according to the temperature measurement result of the temperature measuring thermocouple 47 according to the algorithm, and controls the output power of the furnace electromagnetic induction coil 42 and the sample pool electromagnetic induction coil 44 by changing the PWM (pulse width modulation) output duty cycle; the algorithm for controlling the output pulse signal is specifically as follows:

[0026] (A);

[0027] (B);

[0028] In formulas (A) and (B), is the time occupied by the high pulse signal in one cycle, is the time occupied by the low pulse signal in one cycle, For the cycle, is the input ratio of high pulse signal.

[0029] The temperature measuring thermocouple 47 comprises a furnace cover temperature measuring thermocouple 471, a furnace side temperature measuring thermocouple 472, a furnace bottom temperature measuring thermocouple 473, a sample pool side wall temperature measuring thermocouple 474, and a sample temperature measuring thermocouple 475. The furnace cover temperature measuring thermocouple 471 is inserted into the furnace cover 2 of the adiabatic accelerating calorimeter, the furnace side temperature measuring thermocouple 472 is inserted into the side of the adiabatic accelerating calorimeter furnace body 1, the furnace bottom temperature measuring thermocouple 473 is inserted into the bottom of the adiabatic accelerating calorimeter furnace body 1, and the sample pool side wall temperature measuring thermocouple 474 is inserted into the sample pool 3. The sample temperature measuring thermocouple 475 is inserted into the sample to be tested 33 in the internal space of the sample pool 3; the furnace cover temperature measuring thermocouple 471, the furnace side temperature measuring thermocouple 472, the furnace bottom temperature measuring thermocouple 473, the sample pool side wall temperature measuring thermocouple 474, and the sample temperature measuring thermocouple 475 are respectively used to measure the top temperature of the adiabatic accelerating calorimeter furnace body 1, the side temperature of the adiabatic accelerating calorimeter furnace body 1, the bottom temperature of the adiabatic accelerating calorimeter furnace body 1, the temperature of the sample pool 3, and the temperature of the sample to be tested 33.

[0030] The temperature measuring thermocouples 47 are preferably 6 in number, which are respectively a furnace cover temperature measuring thermocouple 471, a furnace side temperature measuring thermocouple 472, a furnace bottom temperature measuring thermocouple 473, a sample pool side wall temperature measuring thermocouple 474, and a sample temperature measuring thermocouple 475. There are two sample pool side wall temperature measuring thermocouples 474; the two sample pool side wall temperature measuring thermocouples 474 are inserted into the side wall of the sample pool 3.

[0031] The side of the sample pool 3 has two deep holes processed perpendicular to the top of the sample pool 3, the hole diameter is preferably 0.6mm, the hole depth is preferably 16mm, the center positions of the two deep holes are preferably distributed at three equal parts of the side wall thickness, the two deep holes are used to place two sample pool side wall temperature measuring thermocouples 474, and the diameter of each sample pool side wall temperature measuring thermocouple 474 is preferably 0.5mm; the sample pool 3 has a cavity, the cavity includes a feeding channel 31 and a reaction zone 32, the feeding channel 31 is located directly above the reaction zone 32, the feeding channel 31 and the reaction zone 32 are both cylindrical, the inner diameter of the feeding channel 31 is preferably 4.5mm, the wall thickness of the feeding channel 31 is preferably 0.93mm, and the length of the feeding channel 31 is preferably 25mm; preferably, the material of the cylindrical sample pool 3 can be replaced by Hastelloy; the reaction zone 32 is used to place the sample 33 to be tested; the horizontal distances of the center positions of the two deep holes from the center of the sample pool 3 are preferably 14.33mm and 12.67mm respectively.

[0032] The sample temperature measuring thermocouple 475 is inserted from the middle of the sample pool 3 to measure the temperature of the heat released by the reaction of the sample 33 to be tested. The sample pool side wall temperature measuring thermocouple 474 is vertically inserted from the two deep holes at the top of the sample pool 3 until it is inserted into the deepest part of the hole to measure the real-time temperature of the sample pool 3; the temperatures collected by the sample temperature measuring thermocouple 475 and the sample pool side wall temperature measuring thermocouple 474 are displayed and recorded through the human-machine interface of the control software of the computer 49 in the temperature control system 4.

[0033] There is a sample pool heat preservation cotton 7 between the sample pool electromagnetic induction coil 44 and the sample pool 3 ; the sample pool heat preservation cotton 7 is closely attached to the outer wall surface of the sample pool 3 .

[0034] The sample pool 3 is preferably a cylindrical sample pool, and a sample pool electromagnetic induction coil 44 is installed on the outer wall of the cylindrical sample pool. The sample pool electromagnetic induction coil 44 is wrapped around the sample pool thermal insulation cotton 7, and the sample pool electromagnetic induction coil 44 is controlled by an electromagnetic heating controller 46; the sample pool thermal insulation cotton 7 is tightly attached to the outer wall of the sample pool 3; the electromagnetic heating controller 46 is connected to a 220V AC power supply, and the electromagnetic heating controller 46 first rectifies the 220V, 50Hz AC power into DC power, and then converts the DC power into high-frequency high-voltage power with a frequency of 20KHz-40KHz.

[0035] The material of the cylindrical sample pool 3 is preferably stainless steel 316L, the outer diameter of the cylindrical sample pool 3 is preferably 30 mm, the wall thickness of the side of the cylindrical sample pool 3 is preferably 5 mm, and the wall thickness of the top and bottom of the cylindrical sample pool 3 are preferably 2 mm.

[0036] The cylindrical sample pool 3 is located inside the adiabatic accelerating calorimeter furnace body 1 and is connected to the adiabatic accelerating calorimeter furnace cover 2 through a bolt sleeve, and the connection point is the center position of the adiabatic accelerating calorimeter furnace cover 2.

[0037] The sample pool heat preservation cotton 7 is wrapped around the outside of the side wall of the sample pool 3. The thickness of the sample pool heat preservation cotton 7 is preferably 15mm-20mm. The function of the sample pool heat preservation cotton 7 is to ensure that there is a reliable distance between the sample pool electromagnetic induction coil 44 and the sample pool 3 and to keep warm and reduce heat loss. Only a reliable distance can make the various working parameters of the electromagnetic heating controller 46 work normally. If the distance between the sample pool electromagnetic induction coil 44 and the outer wall of the sample pool 3 is too small, the high-frequency current will be very small and the power will not reach the required size. In addition, the sample pool 3 may in turn heat the sample pool electromagnetic induction coil 44, making the sample pool electromagnetic induction coil 44 hot. When the temperature of the sample pool electromagnetic induction coil 44 is too high, its resistance will increase, which is easy to cause its aging and consume more electricity. If the sample If the pool insulation cotton 45 is too thick, that is, the distance between the sample pool electromagnetic induction coil 44 and the outer wall of the sample pool 3 is too large, the voltage on the resonant capacitor in the sample pool electromagnetic induction coil 44 and the electromagnetic heating controller 46 will be higher, and the LC resonant current will also be too large, causing the IGBT module in the electromagnetic heating controller 46 to be burned out; the sample pool electromagnetic induction coil 44 is evenly wound on the sample pool insulation cotton 45, and the interval between each turn of the sample pool electromagnetic induction coil 44 is preferably 5mm when it is wound. The uniform interval ensures that there is no dead point in the heating, ensuring that the sample pool 3 is evenly heated, and the interval between each turn is used to ensure that the sample pool electromagnetic induction coil 44 dissipates heat normally during operation; preferably, the sample pool electromagnetic induction coil 44 preferably uses a mica coil, which can withstand high temperatures of about 500.

[0038] The furnace electromagnetic induction coil 42 and the sample pool electromagnetic induction coil 44 are surrounded by an electromagnetic protection net 45 ; the electromagnetic protection net 45 is a metal mesh structure; the electromagnetic protection net 45 can reduce electromagnetic damage to the human body and the impact of external electric fields on the internal.

[0039] The installation method of the adiabatic accelerating calorimeter furnace body insulation cotton 5 and the furnace body electromagnetic induction coil 42 is the same as the installation operation of the sample pool insulation cotton 7 and the sample pool electromagnetic induction coil 44; the adiabatic accelerating calorimeter furnace body insulation cotton 5 is wrapped around the side wall of the adiabatic accelerating calorimeter furnace body 1, and the furnace body electromagnetic induction coil 42 is wound on the adiabatic accelerating calorimeter furnace body insulation cotton 5 and installed in the furnace body electromagnetic induction coil placement area 6; the adiabatic accelerating calorimeter furnace body insulation cotton 5 is located between the furnace body electromagnetic induction coil 42 and the side wall of the adiabatic accelerating calorimeter furnace body 1; the thickness of the adiabatic accelerating calorimeter furnace body insulation cotton 5 is preferably 15mm-20mm; the furnace body electromagnetic induction coil 42 is evenly wound on the adiabatic accelerating calorimeter furnace body insulation cotton 5, and the interval between each turn of the furnace body electromagnetic induction coil 42 when winding is preferably 5mm.

[0040] The specific working method of the adiabatic accelerating calorimeter based on electromagnetic heating technology includes the following steps:

[0041] 1) Add a certain mass of the sample 33 to be tested and the specific heat capacity is known, insert the sample temperature measuring thermocouple 475 into the sample pool 3, connect the sample pool 3 to the center of the adiabatic accelerating calorimeter furnace cover 2 through bolts, and make the sample pool 3 located in the center of the furnace of the adiabatic accelerating calorimeter furnace body 1 to ensure uniform heating;

[0042] 2) Start by pressing the start button of the control software, the adiabatic accelerating calorimeter based on electromagnetic heating technology enters the heating state, the furnace electromagnetic induction coil 42 and the sample pool electromagnetic induction coil 44 start heating, the sample temperature measuring thermocouple 475 and the sample pool side wall temperature measuring thermocouple 474 respectively measure the temperature of the sample 33 and the sample pool 3, and then transmit the temperature data to the temperature control system 4, and display the temperature data on the configuration interface of the computer 49;

[0043] 3) Compare the temperature rise rate of the tested sample 33 with the preset temperature rise rate threshold; if the temperature rise rate of the tested sample 33 is less than the preset temperature rise rate threshold, it is considered that the tested sample 33 has not yet undergone a chemical reaction, and the preset temperature step value continues to be increased; if the temperature rise rate of the tested sample 33 is greater than or equal to the set temperature rise rate threshold, it is determined that the tested sample 33 is reacting and releasing heat. At this time, the temperature of the tested sample 33 begins to rise continuously, and at the same time, the time proportion of the high pulse signal in a signal cycle is continuously adjusted to change the output power of the furnace electromagnetic induction coil 42 to the absolute value. The furnace body 1 of the thermal acceleration calorimeter is heated to increase the temperature of the furnace body 1 of the adiabatic acceleration calorimeter to track the real-time temperature of the sample 33 to be tested, and try to ensure that the temperature of the furnace body 1 of the adiabatic acceleration calorimeter is consistent with the real-time temperature of the sample 33 to be tested; at the same time, the electromagnetic heating controller 46 intermittently applies excitation pulses to make the electromagnetic induction coil 44 of the sample pool intermittently heated, and controls the intermittent heating time interval to adjust the heating power of the electromagnetic induction coil 44 of the sample pool to heat the sample pool 3, so that the temperature of the sample pool 3 also tracks the real-time temperature of the sample 33 to be tested, and tries to keep the temperature of the sample pool 3 equal to the real-time temperature of the sample 33 to be tested.

[0044] The present invention can utilize electromagnetic heating to heat the sample pool, with higher heating efficiency, faster speed and lower energy consumption, and solves the problem of excessive heat loss and slow heating speed, which causes lag when the adiabatic accelerating calorimeter performs temperature tracking in the thermal runaway stage of chemicals.

[0045] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. Embodiment 1

[0046] The adiabatic accelerating calorimeter using electromagnetic heating described in this embodiment includes an adiabatic accelerating calorimeter furnace body 1, an adiabatic accelerating calorimeter furnace cover 2, a cylindrical sample pool, a temperature control system 4, an adiabatic accelerating calorimeter furnace body insulation cotton 5, a furnace body electromagnetic induction coil placement area 6, and a sample pool insulation cotton 7.

[0047] The cylindrical sample pool 3 is made of stainless steel 316L, with an outer diameter of 30 mm, a wall thickness of 5 mm on the side, and a wall thickness of 2 mm on the top and bottom; the side of the sample pool has two deep holes processed perpendicular to the top of the sample pool, with a hole diameter of 0.6 mm and a hole depth of 16 mm. The positions of the two deep holes are distributed at three equal parts of the side wall thickness, and the two deep holes are used to place two sample pool side wall temperature measuring thermocouples 474 with a diameter of 0.5 mm; there is a cavity in the sample pool 3, including a feeding channel 31 and a reaction zone 32, the feeding channel 31 is located directly above the reaction zone 32, the feeding channel 31 and the reaction zone 32 are both cylindrical, the inner diameter of the feeding channel is 4.5 mm, the wall thickness is 0.93 mm, and the length is 25 mm; preferably, the material of the cylindrical sample pool 3 can be replaced with Hastelloy or titanium alloy.

[0048] The temperature control system 4 includes a 220V AC power supply, a furnace electromagnetic induction coil 42, a temperature measurement module 43, a sample pool electromagnetic induction coil 44, an electromagnetic protection net 45, an electromagnetic heating controller 46, a temperature measurement thermocouple 47, a switch 48 and a computer 49; the cylindrical sample pool 3 is located inside the adiabatic accelerating calorimeter furnace body 1 and is connected to the adiabatic accelerating calorimeter furnace cover 2 by a bolt sleeve, and the connection point is the center position of the adiabatic accelerating calorimeter furnace cover 2; the electromagnetic protection net 45 is a metal mesh structure, which is installed around the furnace electromagnetic induction coil placement area 6 and the sample pool electromagnetic induction coil 44, which can reduce electromagnetic damage to the human body and the influence of the external electric field on the internal.

[0049] In this embodiment, there are 6 temperature measuring thermocouples, namely, furnace cover temperature measuring thermocouple 471, furnace side temperature measuring thermocouple 472, furnace bottom temperature measuring thermocouple 473, sample pool side wall temperature measuring thermocouple 474 and sample temperature measuring thermocouple 475, which are respectively inserted into the adiabatic accelerating calorimeter furnace cover 2, the side of the adiabatic accelerating calorimeter furnace body 1, the bottom of the adiabatic accelerating calorimeter furnace body 1, the side of the sample pool 3 (two), and the sample to be tested 33 in the reaction zone 32 inside the sample pool, respectively measuring the top temperature of the adiabatic accelerating calorimeter furnace body 1, the side temperature of the adiabatic accelerating calorimeter furnace body 1, and the sample to be tested 33 in the reaction zone 32 inside the sample pool. , the bottom temperature of the furnace body 1, the side wall temperature of the sample pool 3 and the temperature of the sample 33; the sample temperature detection thermocouple 475 is inserted from the middle of the sample pool 3 to measure the temperature of the exothermic reaction of the sample 33 to be tested, and the sample pool side wall temperature measuring thermocouple 474 is vertically inserted from the two deep holes on the top of the sample pool 3 until it is inserted into the deepest part of the hole to measure the real-time temperature of the sample pool 3; the temperatures collected by the sample temperature detection thermocouple 475 and the sample pool side wall temperature measuring thermocouple 474 are displayed and recorded through the human-machine interface of the control software of the measurement and control system.

[0050] The adiabatic accelerating calorimeter using electromagnetic heating is characterized in that the electromagnetic heating controller 46 is connected to a 220V AC power supply 41, and is also connected to a furnace electromagnetic induction coil 42 and a sample pool electromagnetic induction coil 44. The electromagnetic heating controller 46 can adjust the power through an IGBT module; the thermocouple 47 is connected to a temperature measurement module 43, and the temperature measurement module 43 converts the current signal of the thermocouple 47 into a digital signal, and outputs it to a computer 49 through a switch 48; the computer 6 outputs a pulse signal to the IGBT module in the electromagnetic heating controller 46 according to an algorithm based on the temperature measurement result of the thermocouple 47, and controls the on and off of the IGBT switch by changing the PWM (pulse width modulation) output duty cycle, thereby controlling the output power of the furnace electromagnetic induction coil 42 and the sample pool electromagnetic induction coil 44.

[0051] The sample pool insulation cotton 7 is wrapped around the side wall of the cylindrical sample pool 3. The thickness of the sample pool insulation cotton 7 is 15mm-20mm. Its function is to ensure that there is a reliable distance between the sample pool electromagnetic induction coil 44 and the sample pool 3 and to keep warm. Only a reliable distance can make the various working parameters of the electromagnetic heating controller 46 work normally. The sample pool electromagnetic induction coil 44 is evenly wound on the sample pool insulation cotton 7. When the coil is wound, the interval between each turn does not exceed 10mm. Preferably, a mica coil is used, which can withstand high temperatures of about 500.

[0052] The specific working method of the adiabatic accelerating calorimeter using electromagnetic heating method includes the following steps:

[0053] 1) Add a certain mass of a sample 33 with a known specific heat capacity to be tested into the cylindrical sample pool 3, insert a sample temperature detection thermocouple 475 into the sample pool 3, install the sample pool 3 to the center of the adiabatic accelerating calorimeter furnace cover 2 through bolt connection, and make the sample pool 3 located in the center of the furnace of the adiabatic accelerating calorimeter furnace body 1 to ensure uniform heating;

[0054] 2) Start by pressing the start button of the control software, the adiabatic accelerating calorimeter enters the heating state, the furnace electromagnetic induction coil 42 and the sample pool electromagnetic induction coil 44 begin to heat, the sample temperature detection thermocouple 475 and the sample pool side wall temperature measurement thermocouple 474 respectively measure the temperature of the sample 33 and the sample pool 3, and then transmit it to the measurement and control system, and display the temperature data on the configuration interface of the computer 49;

[0055] 3) Compare the temperature rise rate of the tested sample 33 with the preset temperature rise detection threshold; if the temperature rise rate of the sample 33 is less than the preset temperature rise rate threshold, increase the preset temperature value; otherwise, it is determined that the sample 33 is reacting and releasing heat. At this time, the temperature of the sample 33 begins to rise continuously, and at the same time, the time proportion of the high pulse signal in a signal cycle is continuously adjusted to change the output power of the furnace electromagnetic induction coil 42 to heat the adiabatic accelerating calorimeter furnace 1, so that the temperature of the adiabatic accelerating calorimeter furnace 1 increases to track the temperature of the sample pool 3, and try to ensure that the temperature of the adiabatic accelerating calorimeter furnace 1 is consistent with the temperature of the sample pool 3; at the same time, excitation pulses are also applied intermittently to heat the sample pool electromagnetic induction coil 44 intermittently, and the intermittent heating time interval is controlled to adjust the heating power of the sample pool electromagnetic induction coil 44 to heat the sample pool 3, so that the temperature of the sample pool 3 also tracks the real-time temperature of the sample 33, and try to keep the temperature of the sample pool 3 equal to the real-time temperature of the sample 33. Embodiment 2

[0056] Preferably, the bottom wall thickness of the cylindrical sample pool 3 is 5 mm, and two deep holes are added on the side wall of the sample pool. The positions of the deep holes correspond to the bottom of the sample pool, and two sample pool bottom temperature measuring thermocouples 476 are inserted into the deep holes until they contact the deepest part of the deep holes; the sample pool bottom temperature measuring thermocouples 476 are used to measure the temperature of the bottom of the sample pool.

[0057] The remaining structures and implementation methods are the same as those in Example 1 and will not be described in detail.

[0058] In summary, the adiabatic accelerating calorimeter using electromagnetic heating proposed in the present invention overcomes the problems of excessive heat loss and slow heating speed caused by the traditional resistance wire heating method. Through the electromagnetic heating method, the sample pool temperature can quickly track the real-time reaction temperature of the sample, so that the reaction environment remains in an adiabatic state. It is generally shown that the present invention has important guiding significance for the effective implementation of reaction safety risk assessment and chemical safety evaluation.

Claims

1. An adiabatic accelerating calorimeter based on electromagnetic heating technology, characterized in that The invention comprises an adiabatic accelerating calorimeter furnace body (1), an adiabatic accelerating calorimeter furnace cover (2), a sample pool (3), a temperature control system (4), an adiabatic accelerating calorimeter furnace body insulation cotton (5), and a furnace body electromagnetic induction coil placement area (6); the sample pool (3) is located inside the adiabatic accelerating calorimeter furnace body (1), the adiabatic accelerating calorimeter furnace cover (2) is located at the furnace body opening of the adiabatic accelerating calorimeter furnace body (1), the adiabatic accelerating calorimeter furnace body insulation cotton (5) is wrapped around the adiabatic accelerating calorimeter furnace body (1), and the furnace body electromagnetic induction coil placement area (6) is located outside the adiabatic accelerating calorimeter furnace body insulation cotton (5); the temperature control system (4) comprises a furnace body electromagnetic induction coil (42) and a sample pool electromagnetic induction coil (44), the furnace body electromagnetic induction coil (42) is installed in the furnace body electromagnetic induction coil placement area (6), and the sample pool electromagnetic induction coil (44) is installed outside the sample pool (3); The temperature control system (4) further comprises an AC power supply (41), a temperature measuring module (43), an electromagnetic protection net (45), an electromagnetic heating controller (46), a temperature measuring thermocouple (47), a switch (48), and a computer (49); the signal input and output ends of the computer (49) are correspondingly connected to the signal output and input ends of the switch (48), the signal input end of the switch (48) is connected to the signal output end of the temperature measuring module (43), the signal input end of the temperature measuring module (43) is connected to the signal output end of the temperature measuring thermocouple (47), and the signal output end of the computer (49) is connected to the first signal input end of the electromagnetic heating controller (46); the computer (49) is used to control heating and display and analyze data; The electromagnetic heating controller (46) includes an IGBT module; the temperature measuring thermocouple (47) is connected to the temperature measuring module (43); the temperature measuring module (43) converts the current signal of the temperature measuring thermocouple (47) into a digital signal, and outputs the digital signal to the computer (49) through the switch (48) using the Modbus TCP communication protocol, and the data is read by the computer (49); the computer (49) controls the output pulse signal to the IGBT module of the electromagnetic heating controller (46) according to the temperature measurement result of the temperature measuring thermocouple (47) and the algorithm, and controls the output power of the furnace electromagnetic induction coil (42) and the sample pool electromagnetic induction coil (44) by changing the PWM output duty cycle; the algorithm for controlling the output pulse signal is specifically as follows: (A)； (B)； In formulas (A) and (B), is the time occupied by the high pulse signal in one cycle, is the time occupied by the low pulse signal in one cycle, For the cycle, is the input ratio of high pulse signal; The sample pool (3) is a cylindrical sample pool, and a sample pool electromagnetic induction coil (44) is installed on the outer wall of the cylindrical sample pool. The sample pool electromagnetic induction coil (44) is wrapped around the sample pool thermal insulation cotton (7), and the sample pool electromagnetic induction coil (44) is controlled by an electromagnetic heating controller (46); the sample pool thermal insulation cotton (7) is tightly attached to the outer wall of the sample pool (3); the adiabatic accelerated calorimeter furnace body thermal insulation cotton (5) is wrapped around the side wall of the adiabatic accelerated calorimeter furnace body (1), and the furnace body electromagnetic induction coil (42) is wrapped around the thermal insulation cotton (7). The accelerating calorimeter furnace body insulation cotton (5) is installed on the furnace body electromagnetic induction coil placement area (6); the adiabatic accelerating calorimeter furnace body insulation cotton (5) is located between the furnace body electromagnetic induction coil (42) and the side wall of the adiabatic accelerating calorimeter furnace body (1); the furnace body electromagnetic induction coil (42) is evenly wound on the adiabatic accelerating calorimeter furnace body insulation cotton (5); the furnace body electromagnetic induction coil (42) and the sample pool electromagnetic induction coil (44) are surrounded by an electromagnetic protection net (45); the electromagnetic protection net (45) is a metal mesh structure.

2. The adiabatic accelerating calorimeter based on electromagnetic heating technology according to claim 1 is characterized in that The power port of the electromagnetic heating controller (46) is connected to the AC power supply (41), the first signal input / output port of the electromagnetic heating controller (46) is connected to the furnace electromagnetic induction coil (42), and the second signal input / output port of the electromagnetic heating controller (46) is connected to the sample pool electromagnetic induction coil (44).

3. The adiabatic accelerating calorimeter based on electromagnetic heating technology according to claim 1 is characterized in that The temperature measuring thermocouple (47) comprises a furnace cover temperature measuring thermocouple (471), a furnace side temperature measuring thermocouple (472), a furnace bottom temperature measuring thermocouple (473), a sample pool side wall temperature measuring thermocouple (474), and a sample temperature measuring thermocouple (475). The furnace cover temperature measuring thermocouple (471) is inserted into the furnace cover (2) of the adiabatic accelerating calorimeter, the furnace side temperature measuring thermocouple (472) is inserted into the side of the adiabatic accelerating calorimeter furnace body (1), the furnace bottom temperature measuring thermocouple (473) is inserted into the bottom of the adiabatic accelerating calorimeter furnace body (1), and the sample pool side wall temperature measuring thermocouple (474) is inserted into the sample pool (3 ), a sample temperature measuring thermocouple (475) is inserted into the sample to be measured (33) in the internal space of the sample pool (3); the furnace cover temperature measuring thermocouple (471), the furnace side temperature measuring thermocouple (472), the furnace bottom temperature measuring thermocouple (473), the sample pool side wall temperature measuring thermocouple (474), and the sample temperature measuring thermocouple (475) are respectively used to measure the top temperature of the adiabatic accelerating calorimeter furnace body (1), the side temperature of the adiabatic accelerating calorimeter furnace body (1), the bottom temperature of the adiabatic accelerating calorimeter furnace body (1), the temperature of the sample pool (3), and the temperature of the sample to be measured (33).

4. The adiabatic accelerating calorimeter based on electromagnetic heating technology according to claim 1 is characterized in that There are six temperature measuring thermocouples (47), which are respectively a furnace cover temperature measuring thermocouple (471), a furnace side temperature measuring thermocouple (472), a furnace bottom temperature measuring thermocouple (473), a sample pool side wall temperature measuring thermocouple (474), and a sample temperature measuring thermocouple (475). There are two sample pool side wall temperature measuring thermocouples (474); the two sample pool side wall temperature measuring thermocouples (474) are inserted into the side wall of the sample pool (3).

5. The adiabatic accelerating calorimeter based on electromagnetic heating technology according to claim 4 is characterized in that The side of the sample pool (3) has two deep holes processed perpendicular to the top of the sample pool (3), with a hole diameter of 0.6 mm and a hole depth of 16 mm. The center positions of the two deep holes are distributed at three equal parts of the side wall thickness. The two deep holes are used to place two sample pool side wall temperature measuring thermocouples (474), and the diameter of each sample pool side wall temperature measuring thermocouple (474) is 0.5 mm. The sample pool (3) has a cavity inside, and the cavity includes a feeding channel (31) and a reaction zone (32). The feeding channel (31) is located directly above the reaction zone (32). The feeding channel (31) and the reaction zone (32) are both cylindrical. The inner diameter of the feeding channel (31) is 4.5 mm, the wall thickness of the feeding channel (31) is 0.93 mm, and the length of the feeding channel (31) is 25 mm.

6. The adiabatic accelerating calorimeter based on electromagnetic heating technology according to claim 4 is characterized in that The sample temperature measuring thermocouple (475) is inserted from the middle of the sample pool (3) to measure the temperature of the reaction heat released by the sample (33) to be tested. The sample pool side wall temperature measuring thermocouple (474) is vertically inserted from the two deep holes at the top of the sample pool (3) until it is inserted into the deepest part of the hole to measure the real-time temperature of the sample pool (3). The temperatures collected by the sample temperature measuring thermocouple (475) and the sample pool side wall temperature measuring thermocouple (474) are displayed and recorded through the human-machine interface of the control software of the computer (49) in the temperature control system (4).

7. The adiabatic accelerating calorimeter based on electromagnetic heating technology according to any one of claims 1 to 6, characterized in that The specific working method of the adiabatic accelerating calorimeter based on electromagnetic heating technology includes the following steps: 1) Add a certain mass of a sample (33) to be tested and having a known specific heat capacity into a sample pool (3), insert a sample temperature measuring thermocouple (475) into the sample pool (3), connect the sample pool (3) to the center of an adiabatic accelerating calorimeter furnace cover (2) through bolts, and make the sample pool (3) located in the center of the furnace of the adiabatic accelerating calorimeter furnace body (1) to ensure uniform heating; 2) Start by pressing the start button of the control software, the adiabatic accelerating calorimeter based on electromagnetic heating technology enters a heating state, the furnace electromagnetic induction coil (42) and the sample pool electromagnetic induction coil (44) begin to heat, the sample temperature measuring thermocouple (475) and the sample pool side wall temperature measuring thermocouple (474) respectively measure the temperature of the sample (33) and the sample pool (3), and then transmit the temperature to the temperature control system (4), and display the temperature data on the configuration interface of the computer (49); 3) Compare the temperature rise rate of the tested sample (33) with a preset temperature rise rate threshold; if the temperature rise rate of the tested sample (33) is less than the preset temperature rise rate threshold, it is considered that the tested sample (33) has not yet undergone a chemical reaction, and the preset temperature step value continues to be increased; if the temperature rise rate of the tested sample (33) is greater than or equal to the preset temperature rise rate threshold, it is determined that the tested sample (33) is undergoing a reaction and releasing heat. At this time, the temperature of the tested sample (33) begins to rise continuously, and at the same time, the time proportion of the high pulse signal in a signal cycle is continuously adjusted to change the output power of the furnace electromagnetic induction coil (42) to give an adiabatic acceleration The calorimeter furnace (1) is heated to increase the temperature of the adiabatic accelerating calorimeter furnace (1) to track the real-time temperature of the sample (33) to be tested, thereby ensuring that the temperature of the adiabatic accelerating calorimeter furnace (1) is consistent with the real-time temperature of the sample (33) to be tested; at the same time, the electromagnetic heating controller (46) intermittently applies excitation pulses to intermittently heat the sample pool electromagnetic induction coil (44), and controls the intermittent heating time interval to adjust the heating power of the sample pool electromagnetic induction coil (44) to heat the sample pool (3), thereby making the temperature of the sample pool (3) also track the real-time temperature of the sample (33) to be tested, thereby keeping the temperature of the sample pool (3) equal to the real-time temperature of the sample (33) to be tested.

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