CN110940692A - Device and method for testing thermal runaway critical parameters of medium-size reaction materials - Google Patents
Device and method for testing thermal runaway critical parameters of medium-size reaction materials Download PDFInfo
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- CN110940692A CN110940692A CN201911199229.1A CN201911199229A CN110940692A CN 110940692 A CN110940692 A CN 110940692A CN 201911199229 A CN201911199229 A CN 201911199229A CN 110940692 A CN110940692 A CN 110940692A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4806—Details not adapted to a particular type of sample
- G01N25/4813—Details not adapted to a particular type of sample concerning the measuring means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4806—Details not adapted to a particular type of sample
- G01N25/4813—Details not adapted to a particular type of sample concerning the measuring means
- G01N25/482—Details not adapted to a particular type of sample concerning the measuring means concerning the temperature responsive elements
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4806—Details not adapted to a particular type of sample
- G01N25/4826—Details not adapted to a particular type of sample concerning the heating or cooling arrangements
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/50—Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility
- G01N25/54—Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility by determining explosibility
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Abstract
The invention discloses a device and a method for testing thermal runaway critical parameters of a medium-sized reaction material. The device makes the material that awaits measuring keep the uniform mixing state through the magnetic stirring of bottom, under homothermal condition, adjusts the rotational speed through rotation and the turbidity sensor of reactor bottom motor, makes the material that awaits measuring keep the uniform mixing state, has realized the simulation to reaction material thermal runaway process actual conditions, solves the problem of the critical parameter test of thermal runaway of evenly stirring liquid reaction system. The reaction runaway critical parameter testing device and the testing method disclosed by the invention can be used for testing the reaction material thermal runaway critical parameters from laboratory magnitude to kilogram level, so that the simulation of the actual conditions of the reaction material thermal runaway process is realized, the accuracy of the testing process is improved, the safety of the testing process is ensured, and the application range of the thermal runaway critical parameter testing device is expanded.
Description
Technical Field
The invention belongs to the field of physical and chemical tests, and relates to a device and a method for testing thermal runaway critical parameters of a medium-size reaction material.
Background
The synthesis of typical energetic compounds often involves a thermal runaway reaction process, the temperature change of the reaction process is severe, and the coupling effect among a temperature field, a velocity field and a concentration field is large. If the process conditions are not properly controlled (too fast feed or not low enough cooling temperature), the heat of reaction can accumulate and accelerate the reaction rate when the heat of reaction cannot be removed effectively. The heat of reaction formation increases exponentially with increasing temperature, while the heat of removal of the reactor on cooling increases only linearly with temperature. Then, when the temperature is further increased, local overheating occurs, which causes reaction runaway and even thermal explosion, and seriously affects life and property safety. Therefore, thermal runaway studies are very important for synthesis reactions.
Most of the synthesis reactions are carried out under isothermal conditions, and the current instruments for isothermal thermal runaway test of the synthesis reactions mainly comprise a micro calorimeter or a test device for researching the thermal explosion of energetic materials, but the device and the method have the following problems: (1) the micro-thermal calorimeter test samples are all milligram-grade, so that the method is suitable for the thermal runaway test of small sample quantity, and the thermal runaway test of synthesis reaction from laboratory magnitude to kilogram-grade can not be carried out; (2) the energetic material thermal explosion testing device is used for testing a static material, is suitable for testing thermal explosion critical parameters of a homogeneous solid or liquid system, and cannot test the thermal explosion critical parameters of the heterogeneous solid or liquid system due to phase separation in the testing process of the heterogeneous (solid-liquid mixing, layering, sedimentation and the like) system.
Disclosure of Invention
In view of the above problems, the present invention provides a critical parameter testing apparatus and method for medium-sized reaction material out-of-control.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a critical parameter testing device for thermal runaway of medium-sized reaction materials comprises a heating unit, a lifting unit, a stirring unit and a detection unit.
The heating unit comprises an alloy bath shell, a heat transfer layer, a heating layer, a heat insulation layer and a shell, wherein the shell, the heat insulation layer, the heating layer, the heat transfer layer and the alloy bath shell are sequentially arranged from outside to inside, and the alloy bath shell is made of aluminum alloy. The periphery of the alloy bath shell is sequentially wrapped with a heat transfer layer, a heating layer, a heat insulating layer and an outer shell from inside to outside.
The lifting unit comprises a lifting arm, a sample adding rod, a worm, a turbine motor assembly and a sample frame, wherein the lower end of the lifting arm is connected with the sample adding rod, the lower end of the extending end of the sample adding rod is vertically connected with the sample frame, and the whole reactor is placed on the sample frame; the worm is installed to the arm internally mounted that takes off and land, and turbine motor assembly is installed to the arm bottom that takes off and land, and turbine motor assembly work makes the arm that takes off and land can drive the application of sample pole and reciprocate together with the reactor through worm up-and-down motion.
The stirring unit comprises a motor, a stirring paddle and a rotor, wherein the stirring paddle is arranged at the upper end of the motor, the rotor is in a rod shape or a shuttle shape and is placed at the bottom of the reactor, the stirring paddle is made of neodymium iron boron materials, and the reactor, the alloy bath shell and the heat insulation layer are arranged between the stirring paddle and the rotor.
The detection unit comprises materials, armored thermocouples, a turbidity sensor, a reactor, a limiting rod, a pressure sensor, a reactor bottleneck, a plug, a connecting wire, an alloy cover and a recorder, wherein the two armored thermocouples are inserted into the materials in the reactor through the plug and are positioned at different positions and different heights from the center in the reactor, and the temperature changes of different positions in the materials are respectively monitored, wherein the reactor is made of pressure-resistant glass, and the plug is made of polytetrafluoroethylene; the plug is in threaded connection with the mouth of the reactor; the reactor is provided with four bottle mouths, two of the bottle mouths are provided with armored thermocouples, one is provided with a turbidity sensor, the turbidity sensor is inserted into the material in the reactor through a plug, the upper position and the lower position of the turbidity sensor are adjusted through a limiting rod in threaded connection with the plug, and the other reactor bottle mouth is in threaded connection with a pressure sensor; the alloy cover is positioned above the alloy bath shell, so that emergency discharge is facilitated when the pressure is too high, the turbidity sensor, the armored thermocouple and the pressure sensor are respectively connected with the recorder through connecting wires, and the recorder records and stores the result of the relevant parameters of thermal runaway of the material in real time.
In order to solve the technical problem, the invention provides a method for testing the thermal runaway critical parameter of a medium-sized reaction material, which comprises the following five steps,
the testing method by utilizing the medium-size reaction material thermal runaway critical parameter testing device comprises the following five steps:
the method comprises the following steps: keeping the reaction temperature of the gold bath shell constant, adding a reaction material into a reactor along the mouth of the reactor, and adding a rotor into the reactor; in the present invention, the reaction mass weight is on the order of hundredths of grams.
Step two: two armored thermocouples, a turbidity sensor and a pressure sensor are screwed on the reactor;
step three: placing the reactor on a sample frame, and placing the reactor into the alloy bath shell by the up-and-down movement of a lifting arm;
step four: turning on a motor to start stirring, and adjusting the rotating speed of a rotor to a rotating speed matched with the actual process material according to the numerical value displayed by the turbidity sensor; specifically, if the value indicated by the turbidity sensor is small, the rotor speed is adjusted to be large, and if the value indicated by the turbidity sensor is large, the rotor speed is adjusted to be small.
Step five: a thermal runaway test was conducted and the temperature, pressure changes over time were recorded.
The beneficial effects of the invention are shown in the following aspects:
(1) the device and the method for testing the thermal runaway critical parameters of the medium-size reaction materials solve the problem that the isothermal thermal runaway parameters of the energetic material synthesis reaction (laboratory magnitude to kilogram level) materials cannot be tested, and the rotation speed is adjusted by the rotation of the motor at the bottom of the reactor and the turbidity sensor, so that the materials to be tested are kept in a uniform stirring state, and the simulation of the actual conditions of the thermal runaway process of the reaction materials is realized.
(2) According to the device and the method for testing the critical parameter of the thermal runaway of the medium-size reaction material, the automatic sample injection of the reaction material is realized through the turbine motor, the dangerous link of sample injection at high temperature is avoided, and the safety of the test process is ensured.
(3) According to the device and the method for testing the thermal runaway critical parameter of the medium-size reaction material, the armored thermocouples at different positions and different heights in the reactor are used for monitoring, so that the test of the internal temperature change of the synthesis reaction material of the energetic material with different magnitudes is realized, the influence of the size effect on the test of the thermal runaway critical parameter of the reaction material is solved, and the test accuracy of the thermal runaway critical parameter of the material is improved.
Drawings
FIG. 1 is a schematic view of the overall configuration of a reaction runaway critical parameter testing apparatus according to the present invention.
1-lifting arm, 2-sample adding rod, 3-alloy bath shell, 4-heat transfer layer, 5-heating layer, 6-heat insulation layer, 7-worm, 8-sample holder, 9-shell, 10-turbine motor component, 11-motor, 12-stirring paddle, 13-rotor, 14-material, 15-armored thermocouple, 16-turbidity sensor, 17-reactor, 18-limiting rod, 19-pressure sensor, 20-reactor bottle mouth, 21-plug, 22-connecting wire, 23-alloy cover, 24-recorder.
FIG. 2 is a graph of the temperature of the center of the reactor over time after thermal runaway of a medium sized reaction mass;
FIG. 3 is a graph of the internal pressure of the reactor over time after thermal runaway of a medium sized reaction mass.
Detailed Description
The present invention will be further described in detail with reference to the accompanying drawings and examples.
As shown in the attached figure 1, the device for testing the thermal runaway critical parameter of the medium-sized reaction material comprises a heating unit, a lifting unit, a stirring unit and a detection unit;
the heating unit comprises an alloy bath shell body 3, a heat transfer layer 4, a heating layer 5, a heat insulation layer 6 and an outer shell 9, wherein the outer shell 9, the heat insulation layer 6, the heating layer 5, the heat transfer layer 4 and the alloy bath shell body 3 are sequentially arranged from outside to inside, and the alloy bath shell body is made of aluminum alloy. The periphery of the alloy bath shell body 3 is wrapped with a heat transfer layer 4, a heating layer 5, a heat insulation layer 6 and an outer shell 9 in sequence from inside to outside.
The lifting unit comprises a lifting arm 1, a sample adding rod 2, a worm 7, a turbine motor assembly 10 and a sample frame 8, wherein the lower end of the extending end of the lifting arm 1 is connected with the sample adding rod 2, the lower end of the sample adding rod 2 is vertically connected with the sample frame 8, and the whole reactor 17 is placed on the sample frame 8; the worm 7 is arranged in the lifting arm 1, the turbine motor component 10 is arranged at the bottom end of the lifting arm 1, the turbine motor component 10 works, and the lifting arm 1 drives the sample adding rod 2 to move up and down together with the reactor 17 through the up-and-down movement of the worm 7.
The stirring unit comprises a motor 11, a stirring paddle 12 and a rotor 13, wherein the stirring paddle 12 is installed at the upper end of the motor 11, the rotor 13 is in a rod shape or a shuttle shape and is placed at the bottom of the reactor 17, the stirring paddle 12 is made of neodymium iron boron materials, and the reactor 17, the alloy bath shell 3 and the heat insulation layer 6 are arranged between the stirring paddle 12 and the rotor 13.
The detection unit comprises two armored thermocouples 15, a turbidity sensor 16, a limiting rod 18, a pressure sensor 19, a reactor bottleneck 20, a connecting wire 22 and a recorder 24, wherein the two armored thermocouples 15 are inserted into the material 14 in the reactor 17 through a plug 21 and are positioned at different positions and different heights from the center in the reactor, and the temperature changes of the different positions in the material are respectively monitored, wherein the reactor is made of pressure-resistant glass, and the plug is made of polytetrafluoroethylene; the plug 21 is in threaded connection with the reactor mouth 20; the reactor 17 has four bottle openings in total, two are provided with armored thermocouples 15, one is provided with a turbidity sensor 16, the turbidity sensor 16 is inserted into the material 14 in the reactor 17 through a plug 21, the upper position and the lower position of the turbidity sensor 16 are adjusted through a limiting rod 18 in threaded connection with the plug 21, and the other reactor bottle opening 20 is in threaded connection with a pressure sensor 19; the alloy cover 23 is positioned above the alloy bath shell 3, so that emergency discharge is facilitated when the pressure is overlarge, the turbidity sensor 16, the armored thermocouple 15 and the pressure sensor 19 are respectively connected with the recorder 24 through the connecting wires 22, and the recorder 24 records and stores the results of the relevant parameters of the thermal runaway of the materials in real time.
The testing method by utilizing the medium-size reaction material thermal runaway critical parameter testing device comprises the following five steps:
the method comprises the following steps: keeping the reaction temperature of the gold bath shell constant, adding a reaction material into a reactor along the mouth of the reactor, and adding a rotor into the reactor; in the present invention, the reaction mass weight is on the order of hundredths of grams.
Step two: two armored thermocouples, a turbidity sensor and a pressure sensor are screwed on the reactor;
step three: placing the reactor on a sample frame, and placing the reactor into the alloy bath shell by the up-and-down movement of a lifting arm;
step four: turning on a motor to start stirring, and adjusting the rotating speed of a rotor to a rotating speed matched with the actual process material according to the numerical value displayed by the turbidity sensor; specifically, if the value indicated by the turbidity sensor is small, the rotor speed is adjusted to be large, and if the value indicated by the turbidity sensor is large, the rotor speed is adjusted to be small.
Step five: a thermal runaway test was conducted and the temperature, pressure changes over time were recorded.
Example 1
The use method of the device is introduced by taking the test of the thermal runaway critical parameter of the reaction material in the heat-preservation final stage of the Ginna synthesis process as an example.
Opening the device, keeping the temperature of the gold bath shell 3 constant to 80 ℃, adding 196g (about 95mL) of heterogeneous reaction material in the final heat-preservation stage of the Ginna synthesis process into a 250mL reactor along the mouth of the reactor when the temperature is stabilized at 80 ℃, and then adding a rotor; two armored thermocouples, a turbidity sensor and a pressure sensor are installed in a screwed mode, the thermocouples are adjusted to be located in different positions (one is close to the wall of the reactor, the other is located in the center of the reactor) and different heights away from the center in the reactor, then the reactor is placed on a sample rack, and the reactor is automatically placed into the alloy bath shell through up-and-down movement of a lifting arm; turning on a motor to start stirring, and adjusting the rotating speed to 450r/min which is matched with the actual process material according to the turbidity sensor; and (5) running a program to perform test testing after the system temperature is stable, and recording the changes of temperature and pressure along with time. The recorded test results are shown in fig. 2 and fig. 3, under the stirring action, the materials in the reactor are homogeneous materials, thermal runaway occurs in about 20min, namely the delay period of the materials at 80 ℃ is 20min, the materials to be tested are kept in a uniform stirring state through the rotation of a motor at the bottom of the reactor, and the simulation of the actual conditions of the thermal runaway process of the reaction materials is realized.
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (6)
1. A critical parameter testing device for thermal runaway of a medium-sized reaction material is characterized by comprising a heating unit, a lifting unit, a stirring unit and a detection unit;
the heating unit comprises an alloy bath shell (3), a heat transfer layer (4), a heating layer (5), a heat insulation layer (6) and an outer shell (9), wherein the heat transfer layer (4), the heating layer (5), the heat insulation layer (6) and the outer shell (9) are sequentially wrapped on the periphery of the alloy bath shell (3) from inside to outside;
the lifting unit comprises a lifting arm (1), a sample adding rod (2), a worm (7), a turbine motor assembly (10), an alloy cover (23) and a sample frame (8), wherein the lower end of the extending end of the lifting arm (1) is connected with the sample adding rod (2), the lower ends of the sample adding rods (2) are respectively and vertically connected with the sample frame (8), and the whole reactor (17) is placed on the sample frame (8); a worm (7) is arranged in the lifting arm (1), a turbine motor component (10) is arranged at the bottom end of the lifting arm (1), the turbine motor component (10) works, and the worm (7) moves up and down to enable the lifting arm (1) to drive the sample adding rod (2) to move up and down together with the reactor (17);
the stirring unit comprises a motor (11), a stirring paddle (12) and a rotor (13), wherein the stirring paddle (12) is arranged at the upper end of the motor (11), the rotor (13) is placed at the bottom of the reactor (17), and the reactor (17), the alloy bath shell (3) and the heat insulation layer (6) are arranged between the stirring paddle (12) and the rotor (13);
the detection unit comprises armored thermocouples (15), turbidity sensors (16), a limiting rod (18), pressure sensors (19) and a recorder (24), the number of reactor mouths (20) is four, the armored thermocouples (15) are installed on two reactor mouths (20), the turbidity sensor (16) is installed on one reactor mouth (20), and the pressure sensor (19) is screwed on the other reactor mouth (20); two armored thermocouples (15) are inserted into the material (14) in the reactor (17) through a plug (21), and the plug (21) is in threaded connection with the reactor mouth (20); the turbidity sensor (16) is inserted into the material (14) in the reactor (17) through a plug (21), the upper and lower positions of the turbidity sensor (16) are adjusted through a limiting rod (18) screwed with the plug (21), and the turbidity sensor (16), the armored thermocouple (15) and the pressure sensor (19) are respectively connected with a recorder (24) through connecting wires (22).
2. The heating unit of claim 1, wherein the alloy bath housing is made of aluminum alloy.
3. The stirring unit of the medium-sized reaction material thermal runaway critical parameter testing device according to claim 1 or 2, wherein the stirring paddle is made of neodymium iron boron material.
4. The reactor of the detecting unit of the medium-sized reaction material thermal runaway critical parameter testing device as claimed in claim 3, wherein the material is made of pressure-resistant glass.
5. The detecting unit for critical parameter testing device of medium size reaction material thermal runaway of claim 4, wherein the plug is made of polytetrafluoroethylene.
6. A test method using the medium-sized reaction material thermal runaway critical parameter test device as set forth in any one of claims 1 to 5, characterized by comprising the steps of:
the method comprises the following steps: keeping the reaction temperature of the gold bath shell constant, adding a reaction material into a reactor along the mouth of the reactor, and adding a rotor into the reactor;
step two: two armored thermocouples, a turbidity sensor and a pressure sensor are screwed on the reactor;
step three: placing the reactor on a sample rack, and automatically placing the reactor into the alloy bath shell by the up-and-down movement of a lifting arm;
step four: turning on a motor to start stirring, and adjusting to a rotating speed matched with the actual process material according to the numerical value displayed by the turbidity sensor;
step five: a thermal runaway test was conducted and the temperature, pressure changes over time were recorded.
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Application publication date: 20200331 |