CN110715873A - Thin combustible pyrolysis temperature and quality synchronous determination experimental system and determination method - Google Patents

Thin combustible pyrolysis temperature and quality synchronous determination experimental system and determination method Download PDF

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CN110715873A
CN110715873A CN201911153675.9A CN201911153675A CN110715873A CN 110715873 A CN110715873 A CN 110715873A CN 201911153675 A CN201911153675 A CN 201911153675A CN 110715873 A CN110715873 A CN 110715873A
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plane mirror
box
plate
temperature
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CN110715873B (en
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龚俊辉
张明锐
王志荣
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Nanjing Tech University
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Nanjing Tech University
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating 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

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Abstract

The invention discloses an experimental system and method for synchronously measuring the pyrolysis temperature and the quality of thin combustible materials, belongs to the technical field of industry, and relates to an experimental device and a method for synchronously measuring the temperature and the quality of a combustible material pyrolysis process. The thermal infrared imager comprises a sample box bracket, a sample box, a gold-plated plane mirror and a thermal infrared imager; the sample box bracket comprises an upper supporting plate, a lower bottom plate and a supporting column; two ends of the supporting column are vertically connected with the upper supporting plate and the lower bottom plate through threads respectively; the upper supporting plate and the lower bottom plate adopt square hard aluminum optical bread boards; the plane mirror base is arranged in the middle of the lower bottom plate, and a gold-plated plane mirror with the inclination consistent with that of the upper plane is fixed on the upper plane; the sample box comprises an outer box and an inner box. The quality measurement and the temperature measurement process of the thermocouple can be carried out simultaneously, separate measurement in different experiments is not needed, the experiment times are reduced, the measured quality and temperature data are guaranteed to be the same sample piece pyrolysis parameters, and the method is particularly suitable for non-ideal uniform materials such as wood.

Description

Thin combustible pyrolysis temperature and quality synchronous determination experimental system and determination method
Technical Field
The invention discloses an experimental system and method for synchronously measuring the pyrolysis temperature and the quality of thin combustible materials, belongs to the technical field of industry, and relates to an experimental device and a method for synchronously measuring the temperature and the quality of a combustible material pyrolysis process.
Background
The solid combustible materials are widely applied in national production and life, and comprise natural and artificial synthetic materials. In particular, synthetic materials such as high molecular polymers have excellent physicochemical properties in marine, land and air transportation tools, business and industrial devices, medical materials, special devices for scientific research, aerospace equipment, sports and leisure and recreation products, and have become important materials in the fields of industry, agriculture, national defense, science and technology, and the like. However, the material is flammable in nature, and is easily pyrolyzed and burned after being heated, and the fire hazard is varied, including heat hazard, smoke hazard, toxic hazard, corrosion hazard, etc., due to the loss of control. With the development of science and technology, various novel polymer materials are increasingly applied to various modern urban buildings (such as building wall thermal insulation materials) due to good physical and chemical characteristics of the polymer materials, but the research on the fire safety of the materials is relatively lagged, and the research comprises pyrolysis kinetic basic research, ignition mechanism, phase change influence (such as thermal deformation, expansion, melting, dripping, gasification and the like), surface fire spreading, environmental influence, fire prevention, flame retardance and the like.
Currently, the most widely used research on the thermal safety of medium-scale materials is the cone calorimeter (ConeCalorimeter) developed by the National Institute of Standards and Technology (NIST) based on the international standard ISO 5660, ASTM E1354, etc., which has been widely used as a standard instrument in various countries around the world. In addition to the conventional mass loss rate and heat release rate during material testing, the surface, internal and backside temperatures associated with material pyrolysis and ignition are also receiving increasing attention from researchers. The conventional temperature measurement generally adopts a K-type thermocouple below 1mm for temperature measurement. The measurement of the mass and the heat release rate are not influenced mutually, but the temperature measurement process of the mass and the thermocouple cannot be carried out simultaneously, and the measurement needs to be carried out in different experiments respectively. Therefore, the method can cause two problems, one is that the number of experiments is doubled, and the measured quality and temperature data can not be ensured to be the pyrolysis parameters of the same sample, especially for non-ideal uniform materials such as wood.
Disclosure of Invention
The invention aims to provide an experimental system and a method for synchronously measuring the pyrolysis temperature and the mass of thin combustible materials, aiming at the defects. The device has scientific and reasonable design, small volume, simple and easy operation, high reliability, wide applicable heat flow range and material variety and high repeatability and acceptance of test results, and completely conforms to the limited heating space of standard instruments such as a cone calorimeter and the like.
The invention is realized by adopting the following technical scheme:
a synchronous measurement experiment system for pyrolysis temperature and quality of thin combustible materials comprises a sample box bracket, a sample box, a gold-plated plane mirror and a thermal infrared imager;
the sample box bracket comprises an upper supporting plate, a lower bottom plate and supporting columns, wherein the upper supporting plate and the lower bottom plate are arranged in parallel; the upper supporting plate and the lower bottom plate are both provided with first threaded holes, both ends of the supporting column are provided with external threads, the threads of the first threaded holes are matched with the external threads, and both ends of the supporting column are respectively vertically connected with the upper supporting plate and the lower bottom plate through threads; the support columns adopt telescopic screws, so that the distance between the upper supporting plate and the lower bottom plate can be conveniently adjusted; the upper supporting plate is a square hard aluminum optical bread board, and a square hole is formed in the middle of the upper supporting plate and provides an optical channel for the thermal infrared imager; the lower bottom plate also adopts a square hard aluminum optical bread board; the number of the support columns is 4;
the plane mirror base is relatively and fixedly arranged in the middle of the lower base plate, the side face of the plane mirror base is a right-angled trapezoid with an upward bevel edge, the upper half part of the plane mirror base is wedge-shaped, the lower half part of the plane mirror base is a screw, an external thread on the screw is matched with a second threaded hole in the lower base plate, an included angle alpha between the upper plane of the plane mirror base and the horizontal plane is 45 degrees, a gold-plated plane mirror with the same inclination as the upper plane is fixed on the upper plane of the plane mirror base, an included angle beta between the mirror face of the gold-plated plane mirror and the horizontal plane is 45 degrees, the reflectivity of the gold-plated plane mirror is greater than 0.97 in;
the sample box comprises an outer box and an inner box, wherein the outer box is a cover-free stainless steel outer box with a square bottom, and a square through hole is formed in the middle of the bottom of the outer box; an inner box is arranged in the outer box, the inner box is divided into an upper plate and a lower plate from top to bottom, the upper plate and the lower plate are both square ceramic fiber plates with square through holes in the middle, the upper plate and the sample piece to be detected are the same in thickness, and the side length of each square through hole is the same as that of the sample piece to be detected; a layer of aluminum net is arranged between the upper plate and the lower plate and used for supporting a sample piece to be tested; aluminum foils are placed at the corresponding positions of the square through holes above the aluminum net to prevent molten materials from dripping from the meshes to pollute the lower components during measurement; black carbon coatings with emissivity larger than 0.95 are coated on the surfaces of the aluminum foil and the aluminum mesh to ensure the measurement precision of the thermal infrared imager;
placing a horizontally fixed thermal infrared imager 10cm away from the center of the mirror surface in the light reflection direction of the gold-plated plane mirror, adjusting the thermal infrared imager to focus on an aluminum foil supporting the bottom of the sample piece, wherein the temperature of the back surface of the sample piece is obtained by measuring the temperature of the aluminum foil in an aluminum grid through the thermal infrared imager, and the parameters of the thermal infrared imager are set according to the emissivity of a carbon coating on the aluminum foil and the radiation law;
the sample box is placed in the center of an upper supporting plate of a sample box support, the sample box support is placed on an electronic balance to measure real-time mass data, and the electronic balance can adopt a commercially available cone calorimeter self-carried electronic balance; the gold-plated plane mirror is positioned between the upper supporting plate and the lower bottom plate, and the thermal infrared imager is horizontal to the central line of the plane mirror, so that the thermal infrared imager can be conveniently focused on the aluminum foil and the aluminum mesh.
Furthermore, in order to conveniently take the sample piece, a handle is fixedly arranged on one side of the sample piece box, and when the sample piece box needs to be moved, the handle is directly moved. The handle is a stainless steel handle, the handle is fixed on the side face of the sample box in a welding mode, the thickness is 1mm, the width is 20mm, and the length is 38 mm.
Furthermore, a second threaded hole is formed in the middle of the lower bottom plate, a screw rod with an external thread is fixed in the middle of the bottom of the plane mirror base, the external thread of the screw rod is matched with the second threaded hole, and the screw rod is screwed into the second threaded hole to fix the plane mirror base on the lower bottom plate.
Furthermore, the plane mirror base is made of hard aluminum material.
Furthermore, the upper plane of the plane mirror base and the gold-plated plane mirror are fixed together by adopting viscose.
Further, the inner diameter of the second threaded hole is 6 mm.
The infrared thermal imager was a commercially available FLIR E40 infrared imager.
Compared with the prior art, the invention has the following advantages:
the mass measurement and the temperature measurement of the thermocouple can be carried out simultaneously, and separate measurement in different experiments is not needed. The experimental frequency can be reduced, and the measured quality and temperature data are ensured to be the pyrolysis parameters of the same sample, especially for non-ideal uniform materials such as wood.
Drawings
The invention will be further explained with reference to the drawings, in which:
FIG. 1 is a front view of a sample pod configuration of the system of the present invention;
FIG. 2 is a top view of the sample cassette of the system of the present invention (without a sample to be tested placed therein);
FIG. 3 is a top view of the sample box structure of the system of the present invention (where the sample to be tested is placed);
FIG. 4 is a schematic diagram of a sample holder, gold plated flat mirrors, and thermal infrared imager configuration of the system of the present invention;
FIG. 5 is a top plan view of the upper plate structure of the sample cassette holder of the system of the present invention;
FIG. 6 is a top view of a lower plate structure of a sample case holder of the system of the present invention;
FIG. 7 is a top view of a gold plated planar mirror structure of the system of the present invention;
FIG. 8 is a schematic view of the system of the present invention in an assembled configuration;
FIG. 9 is a top view of the structure of the system of the present invention in assembled use (without the thermal infrared imager);
FIG. 10 is a bottom view of the base of the system of the present invention in assembled use;
FIG. 11 is a schematic view of the imaging area of the lower surface of the sample photographed by the thermal infrared imager when the system of the present invention is performing measurement;
FIG. 12 is a comparison graph of measured temperatures of the thermal infrared imager and the K-type thermocouple under different heat flows when the system of the present invention performs measurement; wherein, a figure shows 30KW/m2Under heat flow, b shows 50KW/m2Under heat flow, c shows 70KW/m2Flowing down the heat;
FIG. 13 is a graph showing the mass loss rate of samples at different heat flows as measured by the system of the present invention.
In the figure, 1, a sample piece box support, 1-1, an upper supporting plate, 1-2, a lower bottom plate, 1-3, a supporting column, 1-4, a first threaded hole, 2, a sample piece box, 2-1, an outer box, 2-2, an upper plate, 2-3, a lower plate, 2-4, an aluminum net, 2-5, an aluminum foil, 2-6, a screw rod, 2-7, an inner box, 2-8, a second threaded hole, 3, a gold-plated flat mirror, 4, an infrared thermal imager, 5, a flat mirror base, 6, a handle, 7, a sample piece, 8 and an electronic balance.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Referring to fig. 1 ~ 10, the experimental system for synchronously measuring the pyrolysis temperature and the quality of the thin combustible material comprises a sample box bracket 1, a sample box 2, a gold-plated flat mirror 3 and a thermal infrared imager 4.
Referring to the attached drawing 1 ~ 3, a sample box 2 comprises an outer box 2-1 and an inner box 2-7, the outer box 2-1 is a 1mm thick 122mm (external dimension) uncovered stainless steel outer box with a square bottom, the inner box 2-7 is arranged in the outer box 2-1, the inner box 2-7 is divided into an upper plate 2-2 and a lower plate 2-3 from top to bottom, the upper plate 2-2 and the lower plate 2-3 are both square ceramic fiber plates with square through holes in the middle, the upper plate 2-2 and the sample to be measured have the same thickness, the lower plate 2-3 is 10mm thick minus the thickness of the upper plate, the side length of the square through holes is the same as the side length of the sample to be measured, a 0.8mm thick aluminum mesh 2-4 is arranged between the upper plate 2-2 and the lower plate 2-3 for supporting the sample to be measured, a layer of 0.03mm thick aluminum foil 2-5 is arranged at the position corresponding to the square through holes above the aluminum mesh 2-4, molten materials (such as PET, thermal imaging and the like) are placed on the lower part of the aluminum mesh 2-4, and the aluminum foil is coated with the uniform emissivity of a black coating with the emissivity of 95.4, so.
Limited by the size of the heater, the size of the sample piece is not more than 100mm multiplied by 100mm in order to achieve the uniformity of the heat flow on the upper surface of the sample piece. The invention is explained by taking a sample piece with the size of 80mm multiplied by 80mm as an example, the outer box 2-1 adopts a stainless steel shell, if the sample piece with other sizes needs to be tested, only the space (square through hole) for embedding the sample piece in the ceramic fiber board (the upper board and the lower board) in the outer box 2-1 needs to be changed simultaneously, and the sizes of the upper board 2-2 and the lower board 2-3 are both 120mm multiplied by 120 mm. The thermal conductivity and specific heat of the ceramic fiber were 0.06W/mK and 0.67J/gK, respectively. The thickness of the sample piece can be adjusted according to the requirement, and the thickness of the thin combustible material is generally less than 10mm, so 10mm is the upper limit of measurement.
In the testing process, the ceramic fiber plate (the upper plate 2-2 and the lower plate 2-3) is required to be ensured to be in close contact with the stainless steel sample box 2 and the sample without gaps, and the upper surfaces of the ceramic fiber plate, the stainless steel sample box 2 and the sample are parallel and level. In order to conveniently take the sample, a stainless steel handle 6 with the thickness of 1mm, the width of 20mm and the length of 38mm is welded on the right side of the sample box 2, and when the sample box 2 needs to be moved, the handle 6 is directly moved.
Referring to FIG. 4 ~ 10, a sample box 2 is placed on a sample box support 1, the sample box support 1 comprises an upper support plate 1-1, a lower support plate 1-2 and support columns 1-3, the upper support plate 1-1 and the lower support plate 1-2 are arranged in parallel, the upper support plate 1-1 and the lower support plate 1-2 are hard aluminum optical bread boards with the thickness of 1cm and the square of 140mm × 140mm square, the upper support plate 1-1 and the lower support plate 1-2 are both provided with first threaded holes 1-4, both ends of the support columns 1-3 are provided with external threads, the threads of the first threaded holes 1-4 are matched with the external threads, both ends of the support columns 1-3 are respectively and vertically connected with the upper support plate 1-1 and the lower support plate 1-2 through threads, the support columns 1-3 are provided with four stainless steel telescopic screws with the outer diameter of 6mm, the distance between the upper support plate 1-1 and the lower support plate 1-2 is convenient to adjust, the height and the horizontal of the sample box support 1-7 is finally realized by adopting a thermal imaging experiment, the square of the optical bread board 1-2, and the square of the optical bread board is provided with an infrared thermal imaging device, and the square aluminum optical bread board with the size of the square aluminum optical bread board 1-2.
The plane mirror base 5 made of hard aluminum materials is relatively and fixedly arranged in the middle of the lower bottom plate 1-2, an included angle alpha between the upper plane of the plane mirror base 5 and the horizontal plane is 45 degrees, a 2 mm-thick gold-plated plane mirror 3 with the inclination consistent with that of the upper plane is fixed on the upper plane of the plane mirror base 5, an included angle beta between the mirror surface of the gold-plated plane mirror 3 and the horizontal plane is 45 degrees, the size of the gold-plated plane mirror 3 is 140mm multiplied by 130mm, the reflectivity of the gold-plated plane mirror 3 in the wavelength range of 0.8 ~ 10 mu m is larger than 0.97, the waveband comprises most of radiation spectrums, a second threaded hole with the inner diameter of 6mm is formed in the middle of the lower bottom plate 1-2, a screw rod 2-6 with the outer threads and the diameter of 6mm is fixed in the middle of the bottom of the plane mirror base 5, the outer threads of the screw rod 2-6 are matched with the second threaded hole 2-8, the screw rod 2-.
A horizontally fixed thermal infrared imager (FLIR E40) is arranged in the light reflection direction of the gold-plated plane mirror 3 and 10cm away from the center of the mirror surface, the thermal infrared imager 4 is adjusted to be focused on an aluminum foil 2-5 supporting the bottom of a sample, the temperature of the back surface of the sample 7 is obtained by measuring the temperature of the aluminum foil 2-5 in an aluminum mesh 2-4 grid through the thermal infrared imager 4, and the parameters of the thermal infrared imager 4 are set according to the emissivity of a carbon coating on the aluminum foil 2-5 and the radiation law.
When the system is assembled:
firstly, a sample box 2, a sample box bracket 1, a gold-plated plane mirror 3 and a thermal infrared imager 4 are assembled together to form a main body part of the temperature-quality synchronous measurement experimental device. The sample box 2 is located right above the sample box support 1, and the sample box support 1 is placed on an electronic balance 8 (such as a self-contained electronic balance of a cone calorimeter) to measure real-time mass data. The gold plating plane mirror 3 is arranged on a plane mirror base 5 of a lower bottom plate 1-2 of the sample box bracket and is positioned between an upper wrapping plate and a lower wrapping plate (an upper supporting plate 1-1 and a lower bottom plate 1-2). The thermal infrared imager 4 is horizontal to the central line of the gold-plated flat mirror 3 so as to be convenient for focusing on the aluminum foils 2-5 and the aluminum mesh 2-4.
And then placing the sample box 2 prepared with the sample 7 to be detected at the center of the upper supporting plate 1-1 of the sample box bracket 1 to ensure that the hollow part on the back of the sample 7 can be completely monitored by the thermal infrared imager 4. And adjusting the supporting columns 1-3 to enable the height and the level of the sample box bracket 1 to meet the requirements of a determination experiment, namely the distance between the surface of the sample box 2 and the heating source is the required distance. In the adjusting process, the angle between the gold-plated plane mirror 3 and the horizontal plane needs to be ensured to be 45 degrees, then the thermal infrared imager 4 is well arranged according to the fixed distance and height so as to be focused on the aluminum foils 2-5 and the aluminum nets 2-4, and simultaneously the parameter of the thermal infrared imager 4 is ensured to be set as the emissivity of the coatings of the aluminum foils 2-5 and the aluminum nets 2-4.
The system can be used for measuring solid combustible substances such as polymers, wood and the like. This example illustrates the procedure of testing transparent PMMA (Polymethyl Methacrylate) of uniform extruded type with a thickness of 80mm × 80mm and 5 mm. The cutting of sample adopts laser cutting in order to guarantee to be smooth all around, and machine-shaping sample thickness is even, and the thickness error is not more than 0.01mm, and the transparent even impurity-free of material, no obvious bubble, sand hole and aperture. And after the sample piece is cut, placing the sample piece into an oven to be dried for more than 24 hours at 70 ℃ so as to ensure that the surface of the sample piece has no moisture and colloid residues.
When the system is used for the determination experiment, the method comprises the following steps:
1) carrying out temperature calibration;
the temperature of the bottom of the sample piece 7 measured by the thermal infrared imager 4 is compared and calibrated with the temperature of the bottom measured by a traditional thermocouple through a pre-experiment, and the lower surface of the sample piece 7 shot by the thermal infrared imager 4 is divided into three areas, as shown in fig. 11, the peripheral size of the area 1 is 40mm × 40mm, the peripheral size of the area 2 is 60mm × 60mm, the peripheral size of the area 3 is 80mm × 80mm, and the areas of the areas respectively account for 25%, 31.3% and 43.7% of the total area. If the size of the sample changes, the area of each region increases or decreases according to the proportion.
And (3) taking one point in each aluminum grid of the three areas to output the temperature value of each grid at each moment, wherein the average value of the temperatures measured by all the grids in each area is the average temperature in the area. As a result, the average temperature of the three areas is not different from each other by more than 25 degrees before the temperature of the back surface of the sample piece rises to 650K, and the outermost temperature is about 96 percent of the maximum value of the central temperature, and is in an acceptable range, which indicates that the test result is relatively good in one dimension. The main reasons for the difference are the thermal attenuation of the radiation heat flow of the heating cone on the cone calorimeter in the horizontal direction and the edge effect of the sample with limited size, so the average value of the three areas can be used as the back temperature value of the whole sample.
In order to ensure that the thermal infrared imager provides accurate measurement data, a copper plate with the thickness of 3.0 mm and coated with a high-emissivity coating is used for replacing a sample, and 2K-type thermocouples with the diameter of 0.5mm are embedded in the copper plate, so that the temperature difference between the temperature of the thermal infrared imager and the temperature measured by the thermocouples is less than 5K when the temperature of a flat plate rises to 650K. Above 650K, a large systematic difference of about 10K is observed. This difference is due to the reduction in emissivity of the coating (due to its partial degradation).
2) Carrying out a pyrolysis experiment;
2-1) after the sample 7 is placed in the sample box 2, ensuring that the upper surface of the sample 7 is flush with the upper surface of the sample box 2, and then uniformly spraying a black carbon coating with the emissivity of more than 0.95 on the aluminum foil 2-5 and the aluminum grid on the back surface of the sample 7, wherein the thickness of the coating is not more than 0.1 mm;
2-2) placing the whole sample 7 in a drying oven to be dried for more than 24 hours so as to ensure that the coating does not contain moisture;
2-3) the sample box 2 is sent into the assembled system by using the handle 6 of the sample box 2, so that the sample box 2 is horizontally placed on the sample box bracket 1, the bottom of a sample 7 is exposed in the hollow part of the duralumin optical bread board, and only the bottom surface of the sample box 2 is contacted with the sample box bracket 1;
2-4) starting an experiment, wherein the acquisition of experimental data starts from the moment when the sample 7 is exposed to external heat flow, and the synchronism of temperature and quality acquisition needs to be ensured; at 30kW/m2、50kW/m2And 70kW/m2Each experiment was repeated three times under hot flow conditions.
FIG. 12 shows the amount of taper in a master instrument using the set of simultaneous temperature and mass measurement devicesIn the heat meter, the power is 30kW/m2、50 kW/m2And 70kW/m2Bottom temperature profile of PMMA measured under three hot streams. The data points are the average values of three repeated experiments, and the error bars are the credibility ranges of the repeated experiment results. It is obvious that the test result is more stable and the repeatability is higher. Fig. 12 also shows the comparison of the measured temperature values of the thermal infrared imagers and the K-type thermocouples under different heat flows, and it is obvious that the two sets of curves are well matched, which indicates that the bottom temperature of the sample can be measured by the thermal infrared imagers.
Fig. 13 is a graph showing the mass loss rate of a sample measured in a temperature-mass synchronous test experiment, where the data points are the average of three replicates and the error bars are the confidence range of the replicate. It is obvious that the test result of the quality loss is more stable and the repeatability is higher. The experimental device system for the temperature-mass synchronous measurement has higher stability.

Claims (8)

1. The utility model provides a thin combustible substance pyrolysis temperature and quality synchronous measurement experimental system which characterized in that: the thermal infrared imager comprises a sample box bracket, a sample box, a gold-plated plane mirror and a thermal infrared imager;
the sample box bracket comprises an upper supporting plate, a lower bottom plate and supporting columns, wherein the upper supporting plate and the lower bottom plate are arranged in parallel; the upper supporting plate and the lower bottom plate are both provided with first threaded holes, both ends of the supporting column are provided with external threads, the threads of the first threaded holes are matched with the external threads, and both ends of the supporting column are respectively vertically connected with the upper supporting plate and the lower bottom plate through threads; the support columns adopt telescopic screws, so that the distance between the upper supporting plate and the lower bottom plate can be conveniently adjusted; the upper supporting plate is a square hard aluminum optical bread board, and a square hole is formed in the middle of the upper supporting plate and provides an optical channel for the thermal infrared imager; the lower bottom plate also adopts a square hard aluminum optical bread board; the number of the support columns is 4;
the plane mirror base is relatively and fixedly arranged in the middle of the lower base plate, the side face of the plane mirror base is a right-angled trapezoid with an upward bevel edge, the upper half part of the plane mirror base is wedge-shaped, the lower half part of the plane mirror base is a screw, an external thread on the screw is matched with a second threaded hole in the lower base plate, an included angle alpha between the upper plane of the plane mirror base and the horizontal plane is 45 degrees, a gold-plated plane mirror with the same inclination as the upper plane is fixed on the upper plane of the plane mirror base, an included angle beta between the mirror face of the gold-plated plane mirror and the horizontal plane is 45 degrees, the reflectivity of the gold-plated plane mirror is greater than 0.97 in;
the sample box comprises an outer box and an inner box, wherein the outer box is a cover-free stainless steel outer box with a square bottom, and a square through hole is formed in the middle of the bottom of the outer box; an inner box is arranged in the outer box, the inner box is divided into an upper plate and a lower plate from top to bottom, the upper plate and the lower plate are both square ceramic fiber plates with square through holes in the middle, the upper plate and the sample piece to be detected are the same in thickness, and the side length of each square through hole is the same as that of the sample piece to be detected; a layer of aluminum net is arranged between the upper plate and the lower plate and used for supporting a sample piece to be tested; aluminum foils are placed at the corresponding positions of the square through holes above the aluminum net to prevent molten materials from dripping from the meshes to pollute the lower components during measurement; black carbon coatings with emissivity larger than 0.95 are coated on the surfaces of the aluminum foil and the aluminum mesh to ensure the measurement precision of the thermal infrared imager;
placing a horizontally fixed thermal infrared imager 10cm away from the center of the mirror surface in the light reflection direction of the gold-plated plane mirror, and adjusting the thermal infrared imager to focus on an aluminum foil at the bottom of the sample supporting piece;
the sample box is placed in the center of an upper supporting plate of a sample box support, the sample box support is placed on an electronic balance to measure real-time mass data, and the electronic balance can adopt a commercially available cone calorimeter self-carried electronic balance; the gold-plated plane mirror is positioned between the upper supporting plate and the lower bottom plate, and the thermal infrared imager is horizontal to the central line of the plane mirror, so that the thermal infrared imager can be conveniently focused on the aluminum foil and the aluminum mesh.
2. The thin combustible pyrolysis temperature and mass simultaneous determination experimental system according to claim 1, characterized in that: a handle is fixedly arranged on one side of the sample box.
3. The thin combustible pyrolysis temperature and mass simultaneous determination experimental system according to claim 2, characterized in that: the handle is a stainless steel handle, the handle is fixed on the side face of the sample box in a welding mode, the thickness is 1mm, the width is 20mm, and the length is 38 mm.
4. The thin combustible pyrolysis temperature and mass simultaneous determination experimental system according to claim 1 or 2, characterized in that: and a second threaded hole is formed in the middle of the lower bottom plate, a screw rod with external threads is fixed in the middle of the bottom of the plane mirror base, the external threads of the screw rod are matched with the second threaded hole, and the screw rod is screwed into the second threaded hole to fix the plane mirror base on the lower bottom plate.
5. The thin combustible pyrolysis temperature and mass simultaneous determination experimental system according to claim 4, characterized in that: the internal diameter of the second threaded hole is 6 mm.
6. The thin combustible pyrolysis temperature and mass simultaneous determination experimental system according to claim 1 or 2, characterized in that: the plane mirror base is made of hard aluminum material.
7. The thin combustible pyrolysis temperature and mass simultaneous determination experimental system according to claim 1 or 2, characterized in that: the upper plane of the plane mirror base and the gold-plated plane mirror are fixed together by adopting viscose.
8. The method for measuring the thin combustible pyrolysis temperature and quality synchronous measurement experiment system according to claim 1, is characterized by comprising the following steps:
1) carrying out temperature calibration;
1-1) comparing and calibrating the bottom temperature of a sample measured by a thermal infrared imager and the bottom temperature measured by a traditional thermocouple through a pre-experiment, and dividing the lower surface imaging area of the sample photographed by the thermal infrared imager into three areas, wherein the peripheral size of the area 1 is 40mm multiplied by 40mm, the peripheral size of the area 2 is 60mm multiplied by 60mm, the peripheral size of the area 3 is 80mm multiplied by 80mm, and the areas of the areas respectively account for 25%, 31.3% and 43.7% of the total area;
1-2) taking one point in each aluminum grid of the three areas to output a temperature value of each grid at each moment, wherein the average value of the temperatures measured by all the grids in each area is the average temperature in the area;
2) carrying out a pyrolysis experiment;
2-1) after the sample piece is placed in a sample piece box, ensuring that the upper surface of the sample piece is flush with the upper surface of the sample piece box, and then uniformly spraying a black carbon coating with the emissivity of more than 0.95 on the aluminum foil and the aluminum grid on the back surface of the sample piece, wherein the thickness of the coating is not more than 0.1 mm;
2-2) placing the whole sample piece in a drying oven to be dried for more than 24 hours so as to ensure that the coating does not contain moisture;
2-3) sending the sample box into the assembled system by using a sample box handle, ensuring that the sample box is horizontally placed on a sample box bracket and the bottom of the sample is exposed at the hollow part of the duralumin optical bread board, and only the bottom surface of the sample box is contacted with the sample box bracket;
2-4) starting an experiment, wherein the acquisition of experimental data starts from the moment when the sample piece is exposed to external heat flow, and the synchronism of temperature and quality acquisition needs to be ensured; at 30kW/m2、50 kW/m2And 70kW/m2Each experiment is repeated three times under the heat flow working condition;
2-5) taking the average value of the three repeated experiments of the step 2-4) to obtain the measured value of the mass and the temperature of the experimental material.
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