CN210109007U - Experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow - Google Patents
Experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow Download PDFInfo
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- CN210109007U CN210109007U CN201920971400.5U CN201920971400U CN210109007U CN 210109007 U CN210109007 U CN 210109007U CN 201920971400 U CN201920971400 U CN 201920971400U CN 210109007 U CN210109007 U CN 210109007U
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Abstract
The utility model relates to a radiant heating experimental apparatus and polymer pyrolysis test system that catches fire under the device especially relate to a polymer pyrolysis experimental apparatus that catches fire under self-feedback time-varying heat flow. The electric spark torch comprises a base, a heating part, a motor transmission device, a longitudinal support and a control box, wherein the motor transmission device is arranged at the lower part of the base, the longitudinal support is arranged on one side of the upper part of the base, and a baffle rotating rod and an electric spark rotating rod which are vertical to the base are arranged beside the longitudinal support; the baffle rotating rod and the electric spark rotating rod are connected with the base through a rotating shaft; the motor transmission device comprises a motor and a mechanical component thereof; the upper part of the baffle rotating rod is provided with a circular baffle perpendicular to the baffle rotating rod; the heating part comprises a heating cone, a heating cone shell and an electric spark igniter; two first thermocouples are fixedly arranged in the middle of the heating cone and are connected to the control box through holes formed in two sides of the shell of the heating cone; the control box consists of a temperature controller, a baffle switch, an electric spark igniter switch and a heating switch.
Description
Technical Field
The utility model relates to a radiant heating experimental apparatus and polymer pyrolysis test system that catches fire under the device especially relate to a polymer pyrolysis experimental apparatus that catches fire under self-feedback time-varying heat flow.
Background
The pyrolysis ignition of the polymer under the action of external heat flow is the initial stage of the material transformation from the non-ignited state to the ignited state, and is the most critical stage for preventing and controlling the further development of the polymer fire. Experimental study on the polymer pyrolysis ignition process under the radiation heating condition has important significance in the fire risk assessment and control of solid combustible materials.
The conventional polymer pyrolysis ignition experiment and theoretical research mainly focus on the field of normal heat flow. The most commonly used experimental apparatus for standard solid combustible pyrolysis ignition is Cone calorimeter (Cone calorimeter) developed by NIST, national institute of standards and technology, which provides stable heat flow in the range of 0-100kW/m 2. However, in an actual fire scenario, the radiant heat flux received by the unburned materials is typically time-varying, i.e., time-varying, due to changes in fire and flame movement, among other reasons. The heat flow received by the material during the propagation of a Fire at a fixed location has been experimentally determined by researchers and has been shown to increase exponentially with time (S. Manzello et al. Fire Mater, in: 11th International Conference, San Francisco, California, 2009, pp. 215-. The standard instrument cone calorimeter can not realize radiant heat flow which becomes hot continuously along with time, and the research on thermal reaction and thermal safety under the actual heated condition of the polymer is limited to a great extent.
SUMMERY OF THE UTILITY MODEL
The utility model aims at overcoming the limitation that existing standard instrument cone calorimeter etc. can only radiate the invariable thermal current, provide a polymer pyrolysis experimental apparatus that catches fire under the time variant thermal current of self-feedback, be one kind and produce the experimental system of thermal current that changes with time, and carry out the test method that the experiment was surveyed to the pyrolysis of polymer and the process of catching fire under this system. Through a radiation source temperature feedback signal, the output power of a radiation source is regulated by a proportional-integral-derivative controller (PID controller), time-varying heat flow in various forms such as linearity, square, polynomial, exponential, constant, attenuation and the like along with time can be realized, and the pyrolysis ignition test process of various polymers under the heat flow can be completed.
The utility model discloses an adopt following technical scheme to realize:
a polymer pyrolysis ignition experimental device under self-feedback time-varying heat flow comprises a base, a heating component, a motor transmission device, a longitudinal support and a control box, wherein the motor transmission device is arranged at the lower part of the base, the longitudinal support is arranged on one side of the upper part of the base, and a baffle rotating rod and an electric spark rotating rod which are perpendicular to the base are arranged beside the longitudinal support; the baffle rotating rod and the electric spark rotating rod are connected with the base through a rotating shaft and can freely rotate on the base;
the motor transmission device comprises a motor and a mechanical component thereof; the baffle rotating rod rotating shaft is connected with an output shaft of the motor and drives the baffle rotating rod rotating shaft to rotate, so that the baffle rotating rod rotates;
the upper part of the baffle rotating rod is provided with a circular baffle perpendicular to the baffle rotating rod, and the baffle can rotate along with the baffle rotating rod;
the heating part comprises a heating cone, a heating cone shell and an electric spark igniter;
the upper part of the electric spark rotating rod is movably provided with an electric spark igniter perpendicular to the electric spark rotating rod, and the electric spark igniter can rotate along with the electric spark rotating rod; the electric spark igniter is positioned below the baffle;
a heating cone shell is arranged on the longitudinal support at a position higher than the baffle plate, and circular openings are formed in the upper part and the lower part of the heating cone shell; the inner surface of the heating cone shell is provided with a high-temperature-resistant electric insulation ceramic fiber coating; the heating cone shell is conical, a heating cone is arranged in the heating cone shell, the heating cone adopts a heating resistor, and the heating resistor is spirally wound into a cone by a single resistor; the heating cone is fixed in the heating cone shell by adopting a fixed support;
two first thermocouples are fixedly arranged in the middle of the heating cone to measure the real-time temperature of the heating cone, and the first thermocouples are connected to the control box through holes formed in the two sides of the shell of the heating cone;
the control box consists of a temperature controller, a baffle switch, an electric spark igniter switch and a heating switch; the first thermocouple is connected with the temperature controller, a temperature signal of the heating cone is transmitted to the temperature controller to be used as a control signal, and the temperature controller adjusts and controls the power of the heating cone according to the real-time temperature of the heating cone and the temperature of the radiation source corresponding to the set heat flow; the heating cone input power switch, namely the heating switch, is arranged on the control box, and the input power is controlled by the temperature controller; turning on a power switch of the heating cone, heating the heating cone according to a set mode of the temperature controller, stopping heating when the switch is turned off, and losing control of the temperature controller on the heating cone; the motor transmission device is connected with the control box and is powered and controlled by the control box; the baffle switch on the control box controls the rotation and the stop of the baffle rotating rod by controlling the starting and the stop of the motor transmission device; the time for completing the opening or closing action of the baffle is not more than 1s, and when the rotating rod of the baffle rotates, the baffle is far away from the round opening below the heating cone, and the baffle is opened at the moment; when the baffle rotating rod rotates, the baffle blocks the round opening below the heating cone to play a role in heat insulation, and the baffle is closed at the moment; the electric spark igniter is connected with the control box and an electric spark igniter switch on the control box, a 24V power supply is provided by a 220V to 24V transformer in the control box, the electrode distance is 1.5 mm, and the electric spark igniter can be continuously ignited by turning on the electric spark igniter switch; the input power supply of the control box is 220V alternating current power supply.
Furthermore, the electric spark igniter is clamped on the electric spark rotating rod through a clamping clip and can be taken down at any time when the electric spark igniter is not needed.
Furthermore, the length of fixed bolster is 4mm, and the diameter is 20mm, and the fixed bolster adopts high temperature resistant electrical insulation material, and the junction of fixed bolster and heating awl, the internal surface junction of fixed bolster and heating awl shell all adopt insulating welding mode to be connected to guarantee the stability of heating awl.
Further, the heating resistance in the heating cone is coiled into 5 layers, the circumference external diameter of the uppermost layer is 60mm, the circumference external diameter of the lowermost layer is 150mm, and the diameters of the upper opening and the lower opening of the heating cone shell are respectively 60mm and 150 mm.
Furthermore, the distance between the heating cone and the heating cone shell is 5mm, a 4mm thick asbestos fiber protective layer is filled between the heating cone and the heating cone shell, the heat conductivity coefficient of the asbestos fiber is 0.132W/(mK), and electric insulation is realized.
Further, the heating resistor forming the heating cone is a nickel-chromium resistor with the diameter of 10 mm; the rated power of the heating cone is 5000W, and the heat flow output range is 0-100kW/m 2.
Further, the heating cone shell is made of No. 310 stainless steel with the thickness of 3 mm.
The thickness of the high-temperature resistant electrically-insulated ceramic fiber coating on the inner surface of the heating cone shell is 1mm, and the continuous use temperature is 1150 ℃.
Furthermore, the electric spark igniter is positioned 20-25 mm under the baffle.
The utility model also comprises a sample piece bracket, a sample piece box and a sample piece, wherein the sample piece bracket is a height-adjustable bracket with an upper plane and a lower plane; the sample box is made of a polycrystalline mullite fiber heat-insulating material, the heat conductivity coefficient is 0.13W/(mK) at 600 ℃, and the sample box is a cuboid box with a groove on the upper surface; the groove is square or round, and the shape of the groove is determined according to the experiment requirement; the size of the sample piece is consistent with the inner size of the groove, when in test, the sample piece is placed in the groove of the sample piece box, the upper surface of the sample piece is flush with the upper surface of the sample piece box, and the periphery of the sample piece is tightly attached to the inner wall of the groove, so that only the upper surface of the sample piece is exposed;
the middle lower parts of the sample piece and the sample piece box are respectively provided with a second thermocouple hole which is aligned with each other so as to be convenient for placing a second thermocouple, the second thermocouple penetrates through the back surface of the sample piece box and is placed in the sample piece, and the number of the second thermocouples and the depth of the second thermocouples entering the sample piece are determined according to the experiment requirement; the second thermocouple is a K-type thermocouple with the diameter of 0.5 mm.
The sample support comprises an upper surface, a lower surface and a supporting rod, wherein the upper surface and the lower surface are connected through the supporting rod, the supporting rod is a telescopic rod, and the height and the level of the upper surface are adjusted through the matching of a screw rod and a screw.
The baffle comprises an upper layer and a lower layer; the upper layer is a circular asbestos fiber layer with the diameter of 160mm and the thickness of 5mm, the heat conductivity coefficient is 0.132W/(mK), and the upper layer is electrically insulated and 1mm away from the stainless steel shell; the lower layer is stainless steel with the diameter of 160mm and the thickness of 3 mm.
The first thermocouple is a K-type insulated thermocouple with the diameter of 1 mm.
The temperature controller adopts a commercially available Delta DT320 temperature controller.
The utility model discloses the theory of operation of system: the utility model discloses utilize the "feedback-regulation" function of PID controller (proportion-integral-differential controller), according to the real-time difference signal of the last thermocouple actual measurement temperature of installing of heater and target heat flow temperature, the purpose of dynamic adjustment heater output in order to reach the target change heat flow.
Compared with the prior art, the utility model has the advantages of as follows:
1) the power of the heater can be dynamically adjusted according to the real-time feedback signal, the deviation of the output heat flow and the target heat flow is quickly corrected, and higher target heat flow precision can be achieved;
2) compare with the condition that the standard instrument coniform calorimeter can only export invariable thermal current, the utility model discloses a predetermine the PID controller, can realize the time-varying thermal current of multiple variation form, like form thermal current such as linear rising, square rising, exponential rise, linear decline, sectional heating and periodic heating.
The utility model discloses used technique and theory are the maturity method, have built the completion device material object to and cross the actual test of target heat flow calibration and multiple polymer material, the heat flow that its produced agrees with the design heat flow is perfect, heat flow and polymer test experimental result stability and repeatability are high, and test procedure and operating method are simple and easy, and the test result recognition is high.
Drawings
The present invention will be further explained with reference to the accompanying drawings:
FIG. 1 is a schematic diagram of the system of the present invention;
FIG. 2 is a diagram showing the variation of three heat flow patterns for the system to perform target calibration heat flow;
FIG. 3 is a schematic diagram of the calibration of the range of heat flows available to the system;
fig. 4 is a side view of the sample box of the system of the present invention placing a sample to be tested;
fig. 5 is a top view of the sample box of the system of the present invention for placing a sample to be tested;
FIG. 6 is a schematic diagram of the system of the present invention used in temperature measurement and mass loss rate experiments;
FIG. 7 is a graph showing the change of the surface temperature and the internal temperature (3 mm and 6mm in depth) of the sample measured under the linearly rising heat flow when the system of the present invention is used in the temperature measurement and mass loss rate test;
FIG. 8 is a graph showing the results of the loss rate of the system of the present invention for measuring temperature and mass loss rate under linear attenuation heat flow for measuring the surface temperature and the internal temperature (5 mm and 10mm depth);
fig. 9 is the utility model discloses when the system is used for temperature measurement and mass loss rate experiment, actual measurement sample piece mass loss rate result picture under the linear decay heat flow.
In the figure: 1. the device comprises a base, 2, a motor transmission device, 3, a longitudinal support, 4, a control box, 4-1, a temperature controller, 4-2, a baffle switch, 4-3, an electric spark igniter switch, 4-4, a heating switch, 5, a baffle rotating rod, 6, an electric spark rotating rod, 7, a baffle, 8, a heating cone, 9, a heating cone shell, 10, an electric spark igniter, 11, an asbestos fiber protective layer, 12, a fixed support, 13, a first thermocouple, 14, a heat flow meter, 15, a sample piece support (or a balance support), 16, a sample piece box, 17, a sample piece, 18, a second thermocouple, 19, a second thermocouple hole, a type thermocouple of 20 and a type of K, and a vertical distance between the electric spark igniter and the bottom of the heating cone; b. the vertical distance between the heat flux gauge and the bottom of the heating cone.
Detailed Description
The present invention will be described in more detail with reference to the accompanying drawings 1 to 9 and the specific embodiments.
Referring to the attached drawings 1-6, the utility model discloses polymer pyrolysis experimental apparatus that catches fire under time varying heat flow of self-feedback, including base 1, heater block, motor drive 2, longitudinal support 3 and control box 4, motor drive 2 sets up in base 1 lower part, is provided with longitudinal support 3 on one side of base 1 upper portion, is equipped with perpendicular to base 1 baffle bull stick 5 and electric spark bull stick 6 beside longitudinal support 3; the baffle rotating rod 5 and the electric spark rotating rod 6 are connected with the base 1 through rotating shafts and can freely rotate on the base 1; the motor transmission device 2 comprises a motor and mechanical components thereof; the rotating shaft of the baffle rotating rod 5 is connected with the output shaft of the motor to drive the rotating shaft of the baffle rotating rod 5 to rotate, so that the baffle rotating rod 5 rotates; and a circular baffle 7 perpendicular to the baffle rotating rod 5 is arranged at the upper part of the baffle rotating rod 5, and the baffle 7 can rotate along with the baffle rotating rod 5.
The heating part comprises a heating cone 8, a heating cone shell 9 and an electric spark igniter 10;
an electric spark igniter 10 vertical to the electric spark rotating rod 6 is movably arranged at the upper part of the electric spark rotating rod 6, the electric spark igniter 10 is positioned below the baffle 7, and the electric spark igniter 10 can rotate along with the electric spark rotating rod 6.
A heating cone shell 9 is arranged on the longitudinal support 3 at a position higher than the baffle 7, and circular openings are formed in the upper part and the lower part of the heating cone shell 9; the inner surface of the heating cone shell 9 is provided with a high-temperature resistant electric insulation ceramic fiber coating; the heating cone shell 9 is conical, a heating cone 8 is arranged in the heating cone shell 9, the heating cone 8 adopts a heating resistor, and the heating resistor is spirally wound into a cone by a single resistor; the heating cone 8 is fixed in the heating cone shell by adopting a fixed bracket 12; in fig. 1 and 6, the heating resistor in the heating cone 8 has 5 layers, the circumferential outer diameter of the uppermost layer is 60mm, the circumferential outer diameter of the lowermost layer is 150mm, and the diameters of the upper opening and the lower opening of the heating cone shell are respectively 60mm and 150 mm; the fixing bracket 12 is disposed under the 1 st and 4 th floors.
Two first thermocouples 13 are fixedly arranged in the middle of the heating cone 8 to measure the real-time temperature of the heating cone, and the first thermocouples 13 are connected to the control box 4 through holes formed in the two sides of the heating cone shell 9;
the control box 4 consists of a temperature controller 4-1, a baffle switch 4-2, an electric spark igniter switch 4-3 and a heating switch 4-4; the first thermocouple 13 is connected with the temperature controller 4-1, the temperature signal of the heating cone 8 is transmitted to the temperature controller 4-1 as a control signal, and the temperature controller 4-1 adjusts and controls the power of the heating cone 8 according to the real-time temperature of the heating cone 8 and the temperature of a radiation source corresponding to the set heat flow; the input power switch of the heating cone, namely a heating switch 4-4, is arranged on the control box 4, and the input power is controlled by a temperature controller 4-1; turning on a power switch of the heating cone, heating the heating cone 8 according to a set mode of the temperature controller 4-1, stopping heating when the switch is turned off, and losing control of the temperature controller 4-1 on the heating cone 8; the motor transmission device 2 is connected with the control box 4 and is powered and controlled by the control box 4; the baffle switch 4-2 on the control box 4 controls the starting and stopping of the motor transmission device 2 so as to control the rotation and stopping of the baffle rotating rod 5; the opening or closing action completion time of the baffle 7 is not more than 1s, when the baffle rotating rod 5 rotates to enable the baffle 7 to be far away from the circular opening below the heating cone 8, the baffle 7 is opened at the moment; when the baffle rotating rod 5 rotates, the baffle 7 shields the round opening below the heating cone 8 to play a role in heat insulation, and the baffle 7 is closed at the moment; the electric spark igniter 10 is connected with the control box 4 and an electric spark igniter switch 4-3 on the control box 4, a 24V power supply is provided by a transformer which is used for converting 220V into 24V in the control box 4, the electrode distance is 1.5 mm, and the electric spark igniter 10 can be continuously ignited by turning on the electric spark igniter switch 4-3; the input power supply of the control box is 220V alternating current power supply.
The electric spark igniter 10 is clamped on the electric spark rotating rod 6 through a clamping clip, and can be taken down or rotated to a position outside a heating area when the electric spark igniter is not needed; the electric spark igniter 10 is positioned right below the baffle 7, and the vertical distance a between the electric spark igniter and the bottom of the heating cone is 20-25 mm.
Referring to fig. 6, the utility model also has a sample support 15, a sample box 16 and a sample 17, the sample support 15 is a height-adjustable support with upper and lower planes; the sample box 16 is made of a polycrystalline mullite fiber heat-insulating material, the heat conductivity coefficient is 0.13W/(mK) at 600 ℃, and the sample box 16 is a cuboid box with a square groove on the upper surface; the size of the sample piece 17 is the same as the inner size of the groove, when in test, the sample piece 17 is placed in the groove of the sample piece box 16, the upper surface of the sample piece 17 is flush with the upper surface of the sample piece box 16, and the periphery of the sample piece 17 is tightly attached to the inner wall of the groove; the sample box has the function of ensuring that the periphery and the bottom of the sample are in a heat insulation condition, and only the upper surface of the sample is exposed under the calibrated variable heat flow to achieve a one-dimensional heat transfer condition (the condition in the embodiment); according to different experimental conditions, the self-made sample box or the non-used sample box can be used.
Aligned second thermocouple holes 19 are formed in the sample 17 and the lower middle portion of the sample box 16 for receiving second thermocouples 18, the second thermocouples 18 penetrating the back of the sample box 16 and being received in the sample 17, the number of the second thermocouples 18 and the depth of penetration into the sample being determined according to the experiment. The second thermocouple 18 may be a type K thermocouple having a diameter of 0.5 mm.
As shown in fig. 6, the sample holder 15 includes an upper surface, a lower surface and a support rod, the upper surface and the lower surface are connected through the support rod, the support rod is a telescopic rod, and the height and the level of the upper surface are adjusted by matching a screw rod and a screw.
The utility model discloses the test method of device includes following step:
1) calibrating target time-varying heat flow;
2) calibrating the heat flow uniformity of a horizontal plane;
3) and (3) testing the polymer pyrolysis ignition experiment under the time-varying heat flow.
The target time-varying heat flow calibration in the step (1) can realize various time-varying heat flows including linearity, square, polynomial, exponential, constant, attenuation and the like, and each variation mode needs to be set independently.
The target time-varying heat flow calibration comprises three forms of heat flow calibration of natural cooling attenuation, linear descending and linear ascending.
The method for calibrating the natural cooling attenuation heat flow comprises the following steps:
1) after the test system is prepared, a heat flow meter 14 is placed under the heating cone 8, the test surface of the heat flow meter 14 is kept horizontal and is opposite to the heating cone 8, and the vertical distance b between the heat flow meter 14 and the bottom of the heating cone 8 is 30 mm;
2) after the heat flow meter 14 is placed, the power supply of the control box 4 is turned on, the baffle 7 is closed, the control mode of the temperature controller is adjusted to be a PID mode, the SV control mode is set to be a fixed SV mode, and an SV value is set;
3) opening a heating switch to enable the heating cone to start heating; when the temperature of the heating cone rises to a set value SV, opening a baffle, checking a stable heat flow value measured by a heat flow meter, if the measured heat flow value has deviation with a target initial heat flow, adjusting the SV value to make the heat flow measured by the heat flow meter be the target initial heat flow, and recording the SV value and the corresponding heat flow; turning off the heating switch or adjusting the R-S parameter of the temperature controller to STOP in the operation mode, and stopping heating the heating cone; and at the moment, the heat flow measured by the heat flow meter is the natural cooling attenuation heat flow within the time from the beginning to the end of heat flow calibration.
4) And (3) repeating the steps (2) to (3) to calibrate the heat flow for not less than three times, wherein the heat flow change is not more than 5%, and the attenuation change is not more than +/-3 s, and the heat flow calibration is considered to be completed.
The method for calibrating the linear descending heat flow comprises the following steps:
1) switching on a power supply of the master control box, adjusting the control mode of the temperature controller to be a PID mode, setting the SV control mode to be a fixed SV mode, and adjusting the SV value to obtain stable heat flow;
2) in the SV mode, 16 groups of programmable patterns are provided, each group of programmable patterns has 16 steps, each step has two parameters of set temperature SP and set time TM, and the temperature controller controls the heating power of the heating cone to make the real-time temperature of the heating cone reach the set temperature SP within the set time TM; and ensuring the heat flow to be stabilized at the initial heat flow; when the heat flow is stabilized at the initial heat flow, the temperature controller controls the heating cone to cool down, and the heat flow is reduced; fitting heat flow data acquired during the heat flow falling period to obtain an accurate heat flow falling slope; when the heat flow reaches the target and stops the heat flow or the set time is over, stopping calibrating the heat flow; the time from the beginning of the heat flow to the end of the calibration is recorded as the time from the reading of the heat flow meter
The heat flow at the heat flow meter location is a linearly decreasing heat flow, denoted as
；
3) Repeating the calibration heat flow process of the step (2) for not less than three times, if(the time from the beginning of the temperature controller executing step 1 to the time of the heat flow meter reading reaching the target starting heat flow) does not exceed
(in units of seconds) of the reaction mixture,does not vary more than
(in seconds) to obtain a fitting result
If, if
Not less than 0.99, and the change of the falling slope of the linear descending heat flow is not more than
Then the linear decreasing heat flow calibration is completed.
A small unstable region appears just after the heat flow starts to decrease, and the linear degree of the decrease of the heat flow is greatly influenced. At this time, in the course ofSetting the starting step SP00 to be greater than the starting heat flow in the sequence patternAnd recording the time required from the step 1 executed by the temperature controller to the heat flow meter reading reaching the target starting heat flow when calibrating the heat flow, namely the time is the time required by the temperature controller to reach the target starting heat flow
。
The method for calibrating the linear rising heat flow comprises the following steps:
1) switching on a power supply of a master control box, adjusting the control mode of the temperature controller into a PID control mode, calibrating SV initial values and SV ending values corresponding to initial heat flows and ending heat flows in a fixed SV control mode, and editing in a programmable style; unlike the linear decreasing heat flow setting, the heat flow rising does not occur an unstable region, and the set temperature SP00 of the start step in the programmable pattern is directly set to the SV initial value;
2) adjusting the set temperatures SP01 and TM01 in step 1 to change the rising rate of the heat flow; stopping calibration when the heat flow reaches a target and stops the heat flow; the set temperature SP01 is not less than the SV stop value; the time from the beginning of the temperature controller to the end of the heat flow calibration is recorded as
The heat flow measured by the heat flow meter is a linear rising heat flow expressed as
(ii) a Linearly fitting the collected heat flow data to obtain an accurate heat flow rising slope;
3) repeating the calibration heat flow process of the step (2) for at least three times,does not vary more than(unit is second) to obtainTo the fitting resultIf the linear rising heat flow is not less than 0.99, the calibration of the linear rising heat flow is finished;
the correlation between the fitting result and the actual value is expressed, the maximum is 1, and the fitting result is completely consistent with the actual value;
the closer to 1, the higher the fit result fits the actual value.
The target time-varying heat flow calibration method is explained in detail by taking three forms of heat flow calibration, namely natural cooling attenuation, linear descending and linear ascending, as examples, and no spark igniter is needed in the heat flow calibration process.
Example 1 Natural Cooling decay Heat flow setting
1) After the testing system is prepared, referring to fig. 1, a GTT-25-100-RWF model Gardon circular foil type water-cooled heat flow meter 14 (range 0-100kW/m, accuracy 0.001kW/m, response to fig. 1) is horizontally placed right below the heating cone
The reaction time is 80ms, the repeatability is +/-0.5%, the diameter of the radiation receiving target is 12.5 mm, the surface is coated with a durable matt black coating, and the absorptivity is 0.92. The cooling water is room temperature tap water, the flow rate is 13.1 mL/s), the test surface of the cooling water is kept horizontal and is opposite to the radiation source, and the distance from the lower surface of the radiation source stainless steel shell is 30 mm.
2) After the heat flow meter 14 is placed, a power supply of the control box 4 is turned on, the baffle 7 is closed, the control mode of the temperature controller 4-1 is adjusted to be a PID mode (manually set or the temperature controller is automatically adjusted to be a proper PID parameter), an SV (SV represents a set temperature) control mode is set to be a fixed SV mode, and an SV value is set;
3) opening a heating switch 4-4, starting heating the heating cone 8, raising the temperature to a set value, opening a baffle 7, and checking the measurement of a heat flow meter 14The obtained heat flow value. If the heat flow deviates from the target initial heat flow, the SV (set temperature) is adjusted to make the heat flow measured by the heat flow meter be the target initial heat flow (such as
The heat flow corresponds to an SV of 545 ℃ and the SV (set temperature) and the corresponding heat flow are recorded. It should be noted that when the PV (heating coil real-time temperature measurement) displayed on the thermostat 4-1 is just approaching or reaching the target temperature, the heat flow measured by the heat flow meter 14 is not stable, and the heat flow meter 14 should be waiting for the heat flow to be stable (heat flow change)
Regarded as heat flow stable) and then read the heat flow value at the corresponding SV (set temperature). The temperature rise time of the heating cone 8 is 5-8 minutes, and the temperature is stabilized for 20-25 minutes. The heat flow obtained at this time is a normal heat flow, and can be used for experimental study on polymer pyrolysis ignition under the normal heat flow. After the reading of the heat flow meter 14 is stabilized, the heating switch is turned off or the R-S parameter (namely RUN-STOP, which represents the running and stopping parameters of the temperature controller 4-1) in the operation mode of the temperature controller 4-1 is adjusted to be STOP, and the heating cone 8 STOPs heating. At this moment, the heat flow measured by the heat flow meter 14 is the natural cooling decay heat flow within the time (denoted as t decay) from the calibration end of the heat flow.
4) The heat flow is calibrated for not less than three times by repeating the steps (2) to (3), the heat flow change is not more than 5 percent,
not exceeding
(in seconds), the heat flux calibration is considered complete (as in graph a of fig. 2).
Example 2 Linear decreasing Heat flow setting
And (3) switching on a power supply of the master control box, adjusting the control mode of the Delta DT320 temperature controller into a PID mode (can use PID parameters in natural cooling attenuation heat flow setting), setting the SV control mode into a fixed SV mode, and adjusting SV (set temperature) to obtain stable heat flow. Similar to the nominal constant heat flow in the natural cooling decay heat flow setting, the initial and final heat flows of the linearly decreasing heat flow and the corresponding SV initial and SV final values need to be calibrated. The SV control mode is set to the programmable SV mode.
In the SV mode, 16 groups of program patterns are available, each group of program patterns has 16 steps, each step has two parameters of SP (set temperature) and TM (set time), and the temperature controller controls the heating power of the heating cone to make the real-time temperature of the heating cone reach SP in the TM time.
A set of program style editors is arbitrarily selected, SP (here, SP00, SP denotes a set temperature in a programmable style, first 0 denotes a 0 th style, and second 0 denotes a 0 th step) in a start step in the style is set as an SV initial value, and a start step set time (here, TM00, TM00 denotes a set time for heating the radiation source temperature from room temperature to SP00, and if the temperature reaches the set temperature in advance, the remaining time is that the radiation source is stabilized at the set temperature) should be long enough to ensure that the heat flow is stabilized at the initial heat flow. The set temperature SP01 (SP 01 is not greater than SV stop) and the set time TM01 of step 1 were adjusted to change the rate of heat flow decline (the linear rate of heat flow decline is not greater than the natural cooling decline rate). Unlike the set time of step 0, the set time end temperature of step 1 is just changed from SP00 to SP01, and does not reach the set temperature in advance to enter a constant temperature maintaining state. After the style is edited, the SAVE action in the style is executed, and the style is stored in the temperature controller for repeated use. Adjusting the R-S parameter of the operation mode of the DeltaDT320 temperature controller to be STOP, setting the execution mode and the initial step to be 0 and 0 respectively, then setting the R-S parameter to be RUN, and starting the temperature controller to execute the programmable mode 0 from the 0 th step. And adjusting display parameters on a display screen of the Delta DT320 temperature controller as required to set the temperature of the current execution step or the residual execution time of the current execution step. If the SP00 sets the time to end, the heat flow has not risen to the initial heat flow or the heat flow has not stabilized, the R-S parameter RUN → STOP → RUN in the RUN mode can be adjusted to resume the execution of the program pattern, so that the heat flow is stabilized at the initial heat flow (generally 1 to 2 times). Stable heat flowAfter the initial heat flow is determined, the temperature controller executes the step 1 to control the heating cone to cool down, and the heat flow is reduced. Fitting the heat flow data collected during the heat flow ramp down results in an accurate heat flow ramp down slope. When the heat flow is reduced, a small unstable area appears, and the linear degree of the heat flow reduction is greatly influenced. At this time, in the programmable pattern, the set value of the start step SP00 is greater than the SV initial value corresponding to the start heat flow, and the time required from the temperature controller to execute step 1 to the heat flow meter reading to reach the target start heat flow is recorded when the heat flow is calibrated (referred to as "t wait" for short). The heat flow reaches the target stop heat flow or end of the TM01 set time, stopping the calibration heat flow. The time period from the beginning of the heat flow to the end of the calibration of the heat flow is recorded as the reading of the heat flow meter) The heat flow at the position of the heat flow meter is the linear descending heat flow and can be expressed as
. Repeatedly calibrating heat flow not less than three times
Not exceeding
，
The variation does not exceed +/-3 s, and the fitting result
Not less than 0.99, and the change of the falling slope of the linear descending heat flow is not more than
Then the linear decreasing heat flow calibration is considered complete (fig. 2 b).
Example 3 Linear ramp Heat flow setting
In PID control mode (PID parameter manual setting or thermostat automatic control)Dynamic setting), calibrating SV initial values and SV ending values corresponding to the initial heat flow and the ending heat flow in a fixed SV control mode, and editing in a programmable model. Unlike the linearly decreasing heat flow setting, where the heat flow increase does not appear to be in an unstable region, SP00 is set directly to the SV initial value. Adjusting SP01 (SP 01 is no less than SV stop) and TM01 changes the rate of heat flow rise. And stopping the calibration when the heat flow reaches the target and stops the heat flow. From the beginning of the temperature controller to the end of the heat flow calibration (recorded as
) The heat flow measured by the heat flow meter is a linear rising heat flow, which can be expressed as
. The collected heat flow data is linearly fitted to obtain an accurate heat flow rising slope. Repeatedly calibrating the heat flow for at least three times,does not vary more than
(units of seconds), fitting resultsAnd not less than 0.99, the linear ascending heat flow calibration is considered to be completed (as shown in the c diagram of fig. 2).
The system is used for calibrating the heat flow uniformity of the horizontal plane, and the calibration methods of the heat flow uniformity of the horizontal plane with various forms of changes (various forms of changes such as linearity, square, polynomial, exponential, constant, attenuation and the like) are the same, and are uniformly described here.
The method for calibrating the uniformity of the heat flow in the horizontal plane comprises the following steps:
2-1) after the heat flow calibration is finished, keeping the height of the heat flow meter unchanged, moving the heat flow meter to 4 different directions (at a distance of 90 degrees) in a horizontal position respectively, and repeatedly calibrating the heat flow for multiple times;
2-2) when the value measured by the heat flow meter is reduced to 95% of the maximum value of the center, recording the horizontal position of the heat flow meter from the center shaft; the distance from the position to the center point of the measured plane (i.e. the vertical distance b between the heat flow meter and the bottom of the heating cone) is the radius of the available heat flow area (as shown in fig. 3), it is determined that the radii of the available heat flows in 4 different directions of the device are all 35mm, and the size of the sample piece should not be larger than the radius of the available heat flows when the polymer pyrolysis ignition experimental test under the time-varying heat flow is subsequently performed.
The system is used for polymer pyrolysis ignition experimental test under time-varying heat flow, wherein the polymer pyrolysis ignition test parameters comprise surface temperature, internal temperature, mass loss rate and ignition time. Here, taking linear descending and linear ascending heat flow as an example, the specific test method is as follows:
3-1) calibrating target change heat flow;
the electric spark igniter is turned away, a water-cooling heat flow meter is horizontally placed under the heating cone, the upper surface of the heat flow meter is kept horizontal, the distance from the lower surface of the heating cone is 30mm, and stable normal-temperature water flow is introduced into the heat flow meter during the use period to carry out water cooling. The heat flow meter is connected with a 7018 data acquisition module, and the acquisition module is connected to a computer through a data line. The acquisition module is powered by a transformer for converting 220V alternating current into 12V direct current. The data acquisition type of the acquisition module is set as a voltage type, and it needs to be noted that the accuracy of the heat flow data is affected if the set voltage input range is too large. The heat flow output quantity and the heat flow meter measuring range of the experimental device are both
The response of the heat flow meter is
Therefore, the voltage received by the module does not exceed 20mV, so the voltage range of the input data acquisition signal is 0-50 mV. The computer data acquisition program acquires the real-time voltage data of the 7018 module and converts the voltage data into heat flow data according to the responsivity of the heat flow meter, and the acquisition frequency is 1 Hz. And switching on a power supply of the control box, and calibrating the set time-varying heat flow according to a target time-varying heat flow setting method. And opening a computer heat flow acquisition program, and observing whether the heat flow is stable and changes according to a preset mode. Each one of which isThe heat flow working condition is calibrated not less than three times, and the total time error of heat flow change is not more than
(in seconds), heat flow data fitting resultsNot less than 0.99, linear heat flow slope change not more than
. In the whole calibration process, no obvious external airflow interference is required, the environment temperature is stable, and no other heating source interference exists near the heating cone.
3-2) preparing a sample piece to be tested and test equipment;
a polymer material of which the pyrolysis ignition characteristic needs to be measured is selected and processed into blocks (square or round), laser cutting is adopted in all cutting processes, the processed and molded sample piece is uniform in thickness, the thickness error is not more than 0.01mm, the material is uniform, obvious bubbles, impurities, sand holes, small holes, concave-convex shapes, water marks and the like are avoided, the transparency is consistent and good, and the sample piece is called as a sample piece 17 hereinafter. Three to four replicates of each heat flow experiment were performed. The following 50mm square sample is taken as an example for explanation, and the thickness of the sample is selected as required. The sample 17 is placed in a heat insulation sample box 16, the sample box 16 is a polycrystalline mullite fiber heat insulation material, the heat conductivity coefficient is 0.13W/(mK) at 600 ℃, and the specification is 90
90, middle 50
The 50 fretwork places the sample (as figure 4~ 5), and 16 textures of sample box are even, and there are not obvious impurity, defect and unsmooth etc. and the specification error is not more than 0.1 mm. The number of the sample boxes 16 is 4, because the sample boxes 16 are slightly heated during the experiment, and in order to ensure that the next set of experiments are not affected, the sample boxes 16 are cooled to room temperature after each set of experiments, and other cooled sample boxes 16 are used. The sample 17 is put into a sample box 16 for samplingThe periphery of the sample 17 has no obvious gap with the sample box 16, and the upper surface of the sample 17 is horizontal and is flush with the upper surface of the sample box 16. In order to measure the internal temperature of the sample piece, a plurality of round holes (namely, second thermocouple holes 19) with the diameter of 1mm are drilled on the back surfaces of the sample piece 17 and the sample piece box 16 so as to conveniently place the second thermocouples 18, the second thermocouples 18 penetrate through the back surface of the sample piece box 16 and are placed in the sample piece 17, the second thermocouple holes in the sample piece box are aligned with the second thermocouple holes in the back surface of the sample piece, and the quantity of the second thermocouples and the depth of the second thermocouples entering the sample piece are determined according to the experiment requirement. FIG. 4 shows two second thermocouple 18 measuring points with measuring depths of 3mm and 6mm, respectively. The control box power is disconnected, the baffle is closed, the electric spark heater is taken down, the sample support 15 is placed on the base, the sample box 16 is placed on the sample support 15, the height of the sample support 15 is adjusted, the sample 17 is positioned under the heating cone 8, the distance between the upper surface of the sample 17 and the heating cone 8 is 30mm, the levelness of the upper surface of the sample support 15 in multiple directions is measured by a leveling rod, the screw rod of the sample support is adjusted, and the level of the upper surface of the sample support is guaranteed. The temperature of the upper surface of the sample piece 17 is measured by a K-type thermocouple 20 with the diameter of 0.5mm, a probe of the K-type thermocouple 20 is positioned in the center of the upper surface of the sample piece 17 and tightly attached to the upper surface of the polymer, the pressure is not too high, and otherwise the probe of the K-type thermocouple 20 is sunk into the polymer in the pyrolysis stage. Several second thermocouples 18 of the same type measure the internal temperature of the sample piece, ensuring that the probing points of the second thermocouples 18 are always in contact with the bottom surface of the second thermocouple holes 19. The K-type thermocouple 20 and the second thermocouple 18 are connected with another 8-channel 7018 acquisition module, the type of data acquired by the acquisition module is set to be K-type, a computer acquisition program acquires temperature data and records acquisition time, the accuracy of the temperature data is 0.1 ℃, and the acquisition frequency is 1 Hz. In order to measure the mass loss rate in the pyrolysis process, the sample piece support 15 in the temperature measurement experiment is taken down, an electronic balance with a balance support is placed on the sample piece support, and the electronic balance with the measuring range of 0.001g and 10 kg is placed on a stainless steel base. A light fireproof plate with the thickness of 1cm is placed on the electronic balance to heat the balance through a fireproof heating cone. The height of the balance support is adjusted to enable the upper surface of the sample piece 17 to be 3cm away from the lower surface of the heating cone 8, and the level gauge on the electronic balance is adjusted to enable the balance to be horizontal. The electronic balance is connected to a computer through a data line, and an acquisition program acquiresReal-time quality data, acquisition frequency 1 Hz. The pyrolysis mass loss rate experimental schematic is shown in fig. 6. It should be noted that the connection between the type K thermocouple 20 and the second thermocouple 18 may prevent the electronic balance from accurately measuring the mass data, and therefore, the thermometry experiment and the mass measurement experiment should be separately performed.
3-3) determining the pyrolysis ignition experiment of the polymer;
and (4) closing the baffle 7, switching on a power supply of the control box, and setting parameters of the temperature controller according to the setting method of the calibration heat flow in the step (1). When the heat flow starts to change, the baffle 7 under the heating cone 8 is opened and simultaneously the data acquisition program is opened to start the experiment. The data acquisition program records experimental time and real-time temperature data (including surface and internal temperatures) or mass data throughout the experiment. And (3) stopping the data acquisition program immediately after the stable flame appears on the surface of the sample piece 17 or the experiment time exceeds the heat flow calibration time, terminating the experiment and closing the baffle. And repeating the experiment twice or three times without changing the target change heat flow, wherein the average value of the parameters measured by multiple experiments is the target parameter measured in the pyrolysis ignition process of the polymer. After many experiments, the baffle temperature will rise. In the experiment preparation stage, the baffle in the closed state can heat the sample piece in a small range, the experiment is suspended, the heating switch is closed, and the cooling baffle is cooled to the room temperature to continue the next group of experiments. And selecting different time-varying heat flows, and repeating the experimental steps to obtain the change rules of the time-varying heat flows in different forms and the pyrolysis ignition characteristics of the material to be detected under the heat flows.
Fig. 7 shows the measured changes in the surface and internal temperatures (3 mm and 6mm depth) of a PMMA (Poly methyl methacrylate) sample under a typical linearly rising heat flow, illustrating the faster the heat flow rate, the faster the temperature rise, and the shorter the ignition time.
FIG. 8 shows the measured surface temperature, internal temperature (5 mm and 10mm depth) loss rate results for PMMA samples under typical linear decay heat flow; FIG. 9 shows the mass loss rate results for PMMA samples measured under typical linear decay heat flow. It is shown that the slower the heat flow decay rate, the faster the surface temperature rise, the faster the mass loss and the shorter the ignition time.
Claims (9)
1. The utility model provides a polymer pyrolysis experimental apparatus that catches fire under time-varying heat flow of self-feedback which characterized in that: the electric spark torch comprises a base, a heating part, a motor transmission device, a longitudinal support and a control box, wherein the motor transmission device is arranged at the lower part of the base, the longitudinal support is arranged on one side of the upper part of the base, and a baffle rotating rod and an electric spark rotating rod which are vertical to the base are arranged beside the longitudinal support; the baffle rotating rod and the electric spark rotating rod are connected with the base through a rotating shaft and can freely rotate on the base;
the motor transmission device comprises a motor and a mechanical component thereof; the baffle rotating rod rotating shaft is connected with an output shaft of the motor and drives the baffle rotating rod rotating shaft to rotate, so that the baffle rotating rod rotates;
the upper part of the baffle rotating rod is provided with a circular baffle perpendicular to the baffle rotating rod, and the baffle can rotate along with the baffle rotating rod;
the heating part comprises a heating cone, a heating cone shell and an electric spark igniter;
the upper part of the electric spark rotating rod is movably provided with an electric spark igniter perpendicular to the electric spark rotating rod, and the electric spark igniter can rotate along with the electric spark rotating rod; the electric spark igniter is positioned below the baffle;
a heating cone shell is arranged on the longitudinal support at a position higher than the baffle plate, and circular openings are formed in the upper part and the lower part of the heating cone shell; the inner surface of the heating cone shell is provided with a high-temperature-resistant electric insulation ceramic fiber coating; the heating cone shell is conical, a heating cone is arranged in the heating cone shell, the heating cone adopts a heating resistor, and the heating resistor is spirally wound into a cone by a single resistor; the heating cone is fixed in the heating cone shell by adopting a fixed support;
two first thermocouples are fixedly arranged in the middle of the heating cone to measure the real-time temperature of the heating cone, and the first thermocouples are connected to the control box through holes formed in the two sides of the shell of the heating cone;
the control box consists of a temperature controller, a baffle switch, an electric spark igniter switch and a heating switch; the first thermocouple is connected with the temperature controller, a temperature signal of the heating cone is transmitted to the temperature controller to be used as a control signal, and the temperature controller adjusts and controls the power of the heating cone according to the real-time temperature of the heating cone and the temperature of the radiation source corresponding to the set heat flow; the heating cone input power switch, namely the heating switch, is arranged on the control box, and the input power is controlled by the temperature controller; the motor transmission device is connected with the control box and is powered and controlled by the control box; a baffle switch on the control box controls the starting and stopping of the motor transmission device; the electric spark igniter is connected with the control box and an electric spark igniter switch on the control box.
2. The experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow according to claim 1, wherein: the heating resistance in the heating cone is coiled into 5 layers, the circumference external diameter of the uppermost layer is 60mm, the circumference external diameter of the lowermost layer is 150mm, and the diameters of the upper opening and the lower opening of the heating cone shell are respectively 60mm and 150mm correspondingly.
3. The experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow according to claim 1, wherein: the length of fixed bolster is 4mm, and the diameter is 20mm, and the fixed bolster adopts high temperature resistant electrical insulation material, and the junction of fixed bolster and heating awl, the internal surface junction of fixed bolster and heating awl shell all adopt insulating welding mode to be connected to guarantee the stability of heating awl.
4. The experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow according to claim 1, wherein: the distance between the heating cone and the heating cone shell is 5mm, and a 4mm thick asbestos fiber protective layer is filled between the heating cone and the heating cone shell.
5. The experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow according to claim 1, wherein: the electric spark igniter is clamped on the electric spark rotating rod through the clamp, and can be taken down at any time when the electric spark igniter is not needed.
6. The experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow according to claim 1, wherein: the baffle comprises an upper layer and a lower layer; the upper layer is a circular asbestos fiber layer with the diameter of 160mm and the thickness of 5 mm; the lower layer is stainless steel with the diameter of 160mm and the thickness of 3 mm.
7. The experimental apparatus for polymer pyrolysis ignition under self-feedback time-varying heat flow according to claim 1, wherein: the system also comprises a sample piece bracket, a sample piece box and a sample piece, wherein the sample piece bracket is a height-adjustable bracket with an upper plane and a lower plane; the sample box is a cuboid box with a groove on the upper surface; the size of the sample piece is the same as that of the inner wall of the groove; during testing, the sample piece is placed in the groove of the sample piece box, the periphery of the sample piece is tightly attached to the inner wall of the groove, and the upper surface of the sample piece is flush with the upper surface of the sample piece box, so that only the upper surface of the sample piece is exposed;
and aligned second thermocouple holes are formed in the middle lower parts of the sample piece and the sample piece box so as to place a second thermocouple, and the second thermocouple penetrates through the back surface of the sample piece box and is placed in the sample piece.
8. The apparatus of claim 7, wherein the apparatus comprises: the sample support comprises an upper surface, a lower surface and a supporting rod, the upper surface and the lower surface are connected through the supporting rod, and the supporting rod is a telescopic rod.
9. The apparatus of claim 7, wherein the apparatus comprises: the groove is square or round.
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| CN110108752B (en) * | 2019-06-26 | 2024-04-09 | 南京工业大学 | Polymer pyrolysis ignition experimental system under self-feedback time-varying heat flow and testing method |
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