CN113533240A - Solid particle measuring device and method in pyrolysis process - Google Patents
Solid particle measuring device and method in pyrolysis process Download PDFInfo
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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Abstract
The invention discloses a solid particle measuring device and method in a pyrolysis process. The method comprises the steps that a substance to be measured is burnt in an absorption cell, photographing equipment is matched with the absorption cell to photograph the burning state of the substance to be measured, a reflecting element is arranged in the absorption cell, infrared light emitted by an infrared laser passes through the lens to form infrared light refracted light and infrared light reflected light by utilizing an infrared laser, a lens, a first infrared light detector and a second infrared light detector, the infrared light reflected light is received by the first infrared light detector, the infrared light refracted light is incident into the absorption cell and is reflected for multiple times by the reflecting element in the absorption cell, and then the infrared light refracted light is emitted out of the absorption cell and is received by the second infrared light detector. The invention solves the problem of synchronously measuring the physical form and key components of the solid particles in the fast pyrolysis process, obtains clear flame form and high-time-resolution gas-phase components, and synthesizes the two results to research the combustion characteristics of the solid particles in the fast pyrolysis process.
Description
Technical Field
The invention relates to the field of optical detection, in particular to a solid particle measuring device and method in a pyrolysis process.
Background
Fast pyrolysis is one of the main routes for converting solid fuels to liquid fuels, and it requires that the sample be heated rapidly (at a heating rate in excess of 1000K/min) at higher temperatures (450 ℃ to 600 ℃) and with residence times typically less than 2 seconds to obtain liquid bio-oil products up to 75 wt%. Despite advances in biomass fast pyrolysis technology, there are still advancesThere is a problem of not being economical enough, and the large-scale commercial application has a long way to go. The vague knowledge of the chemical and physical changes that occur during the fast pyrolysis of solid fuels limits the further development of fast pyrolysis technology. The time scale of fast pyrolysis is usually in the order of sub-seconds, and Dauenhauer et al obtain the phase change of cellulose during fast pyrolysis with a high-speed camera (1000 frames/second), record the process of infiltrating the heating surface with the intermediate liquid, and preliminarily establish a heat transfer and aerosol formation model in the pyrolysis process according to experimental results. The solid fuel is accompanied by the breaking of old chemical bonds and the formation of new chemical bonds while undergoing processes such as phase change, gasification and the like. Because this process is so rapid that it is difficult to capture the product information therein, researchers' knowledge of the chemical changes therein remains elusive. The permanent gas products generated by pyrolysis comprise CO and CO2、H2O、H2And the like. Accurate, real-time measurement of these major gas phase products is key to constructing fast pyrolysis mechanisms and models. The gas chromatography can be used as a separation and qualitative means to perform more accurate qualitative and quantitative analysis on the gas product, but can only acquire the average information of the product within tens of minutes. Mass spectrometry as a detector can improve the time resolution of product analysis, however millisecond resolution is also typically not achieved. In recent years, Tunable Diode Laser Absorption Spectroscopy (TDLAS) technology is widely used in the field of solid fuel conversion, and millisecond-level time resolution can be realized by using high-frequency Laser as a light source, so that products of a pyrolysis process can be rapidly diagnosed. In order to clearly recognize the chemical and physical changes in the fast pyrolysis process of the solid fuel, it is necessary to develop a device and a method capable of synchronously measuring the physical form and key components of solid particles in the fast pyrolysis process, so as to complete the academic research and accelerate the large-scale commercialization of the fast pyrolysis technology of biomass.
Disclosure of Invention
The invention aims to provide a device and a method capable of synchronously measuring the physical form and key components of solid particles in a fast pyrolysis process.
In order to achieve the above object, the present invention provides a solid particle measuring device in pyrolysis process for measuring physical form and composition of solid particles in pyrolysis process, the measuring device comprises an absorption cell, a photographic device, an infrared laser, a lens, a first infrared detector and a second infrared detector,
the absorption cell is used for burning a substance to be measured and is provided with a reflecting element, and the photographic equipment is matched with the absorption cell and is used for photographing the burning state of the substance;
the infrared laser, the lens, the first infrared light detector and the second infrared light detector are arranged in such a way that infrared light emitted by the infrared laser passes through the lens to form infrared light refraction light and infrared light reflection light, the infrared light reflection light is received by the first infrared light detector, and the infrared light refraction light enters the absorption cell and is reflected out of the absorption cell after being reflected for multiple times by the reflecting element in the absorption cell and is received by the second infrared light detector.
In one embodiment, the measuring device comprises at least one mirror mounted on the optical path of the infrared light reflected light and/or the infrared light refracted light and adapted to change the propagation direction of the infrared light reflected light and/or the infrared light refracted light.
In one embodiment, the side wall of the absorption tank is provided with at least one perspective window, and the photographic equipment is arranged on the outer side of the perspective window and matched with the perspective window to photograph the combustion state of the substances in the absorption tank.
In one embodiment, the measuring apparatus further includes a first reflecting mirror disposed on an entrance optical path of the absorption cell and adapted to change a traveling direction of the infrared light refracted light exiting from the lens, a second reflecting mirror disposed on an entrance optical path of the first infrared light detector and adapted to change a traveling direction of the infrared light reflected by the lens, and a third reflecting mirror disposed on an exit optical path of the absorption cell and adapted to change a traveling direction of the light exiting from the absorption cell.
In one embodiment, the measuring device further includes a visible light laser, light emitted by the visible light laser forms visible light reflected light and visible light refracted light after passing through the lens, the visible light reflected light coincides with the infrared light refracted light, and the visible light refracted light coincides with the infrared light reflected light.
In one embodiment, the measuring apparatus further includes a fourth mirror disposed on an exit optical path of the visible laser and configured to change a propagation direction of the visible light entering the lens, a plurality of fifth mirrors disposed between the lens and the absorption cell and configured to change a propagation direction of the light from the lens to the absorption cell, a sixth mirror disposed on an exit optical path of the absorption cell and configured to change a propagation direction of the light from the absorption cell to the second infrared light detector, and a seventh mirror disposed on an entry optical path of the first infrared light detector and configured to change a propagation direction of the light reflected by the lens.
In one embodiment, the absorption pool is internally provided with a first cylindrical mirror and a second cylindrical mirror which are oppositely arranged in the absorption pool and are respectively positioned on an inlet light path and an outlet light path of the absorption pool, wherein the first cylindrical mirror is provided with a light ray inlet, the second cylindrical mirror is provided with a light ray outlet, and light entering the absorption pool passes through the light ray inlet and then passes through the light ray outlet to leave the absorption pool after being reflected for multiple times between the first cylindrical mirror and the second cylindrical mirror.
In one embodiment, the projections of the reflective surfaces of the first cylindrical mirror and the second cylindrical mirror are arranged on the same circle.
In one embodiment, the first cylindrical mirror and the second cylindrical mirror are both square cylindrical mirrors with the side length between 50mm and 200mm and the curvature radius of 400 mm.
In one embodiment, the measuring device further comprises a heater disposed in the absorption cell for heating a substance to be measured; preferably, the heater is a silicon carbide heating plate.
In one embodiment, the heater is disposed between the first cylindrical mirror and the second cylindrical mirror, and is preferably disposed at a central position of the first cylindrical mirror and the second cylindrical mirror.
In one embodiment, the measuring device further comprises a temperature controller connected to the heater circuit for regulating the temperature of the heater.
In one embodiment, the measuring device further comprises a feed pipe arranged vertically above the heater, from which feed pipe the substance to be measured enters the absorption cell by gravity.
In one embodiment, the feed tube is a quartz tube.
In one embodiment, the measurement device further comprises a data acquisition unit in signal connection with the first infrared light detector and the second infrared light detector respectively to collect absorption spectrum signals acquired by the first infrared light detector and the second infrared light detector.
In one embodiment, the data acquisition unit is a data acquisition card.
In one embodiment, the measuring apparatus further comprises a data processing unit in signal connection with the data acquisition unit and the photographing device.
In one embodiment, the shutter speed of the photographic device is in the range of 1000 and 100000 frames/second.
In one embodiment, the frequencies of the infrared reflected light and the infrared refracted light collected by the first infrared light detector and the second infrared light detector are in the range of 10000-.
A second object of the invention is to provide a method for measuring the morphology and composition of solid particles in a pyrolysis process, said method comprising the steps of:
step S1: heating a substance to be measured by using a heater;
step S2: infrared light is utilized to form infrared light refracted light and infrared light reflected light through a lens, the infrared light reflected light is adjusted to be received by a first infrared light detector, and the adjusted infrared light refracted light is adjusted to be received by a second infrared light detector after passing through a reaction area for heating a substance to be measured;
step S3: the reaction area is photographed using a photographing apparatus.
Preferably, the step S1, the step S2 and the step S3 are performed simultaneously.
In one embodiment, the method further comprises:
step S4: performing light path modulation on the infrared refraction light and the infrared reflection light by using visible light;
preferably, in step S4, visible light is used to form visible light refracted light and visible light reflected light after passing through the lens, the visible light refracted light is adjusted to coincide with the infrared light reflected light optical path, the visible light reflected light is adjusted to coincide with the infrared light refracted light optical path, and the visible light reflected light is adjusted to reach the second infrared light detector after passing through the reaction region.
In one embodiment, in step S2, a first cylindrical mirror and a second cylindrical mirror are disposed on two opposite sides of the reaction region, and an aperture is disposed on each of the first cylindrical mirror and the second cylindrical mirror, and the optical path of the infrared refracted light is adjusted such that the infrared refracted light enters the reaction region through the aperture of the first cylindrical mirror and is received by the second infrared light detector after being emitted through the aperture of the second cylindrical mirror after being reflected between the first cylindrical mirror and the second cylindrical mirror for multiple times.
In one embodiment, in the step S2, the optical path of the infrared light refracted light is adjusted such that the infrared light refracted light is reflected at least five times on the first cylindrical mirror and the second cylindrical mirror, respectively.
In one embodiment, in the step S3, the shutter speed of the photographing device for acquiring the image information is adjusted to be in the range of 1000 and 100000 frames/second.
In one embodiment, in the step S2, the frequencies of the first infrared light detector and the second infrared light detector for collecting the reflected infrared light and the refracted infrared light are adjusted to be within the range of 10000-.
In one embodiment, in the step S1, the substance to be measured is heated by a heater, and the heater is adjusted to be preheated to a temperature range of 700-.
In one embodiment, the method further comprises collecting absorption spectrum signals collected by the first infrared light detector and the second infrared light detector simultaneously with a data collection unit.
The invention provides a device and a method for measuring the physical form and key components of solid particles in a fast pyrolysis process, which can measure the transient combustion process and the release rule of gas-phase products on a millisecond time scale. The method overcomes the defect that the modulation of the optical path is too complex in the traditional measurement technology, the optical paths of the visible light and the infrared light used for the experiment are superposed by introducing the collimated coupling of the visible light and the infrared light, and the visible light is used for replacing the infrared light to modulate the complex optical path, so that the measurement process is simpler and more accurate. The synchronous measuring device is simple and easy to build, high in reliability, rich in measuring information, high in speed and high in accuracy, and is very suitable for academic research and industrial application.
Drawings
FIG. 1 is a schematic diagram of an apparatus for simultaneously measuring the physical form and key components of solid particles in a fast pyrolysis process according to one embodiment of the present invention.
Fig. 2 is a cross-sectional view of the embodiment of fig. 1 taken at the center of the cell.
FIG. 3 is a schematic diagram of an apparatus for simultaneously measuring the physical form and key components of solid particles in a fast pyrolysis process according to another embodiment of the present invention.
FIG. 4 shows measured CO from pyrolysis of corn cobs in an embodiment of the present invention2Release profile and particle morphologyThe process of variation of (c).
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the objects, features and advantages of the invention can be more clearly understood. It should be understood that the embodiments shown in the drawings are not intended as limitations on the scope of the invention, but are merely illustrative of the true spirit of the technical solutions of the present invention.
In the following description, for the purposes of illustrating various disclosed embodiments, certain specific details are set forth in order to provide a thorough understanding of the various disclosed embodiments. One skilled in the relevant art will recognize, however, that the embodiments may be practiced without one or more of the specific details. In other instances, well-known devices, structures and techniques associated with this application may not be shown or described in detail to avoid unnecessarily obscuring the description of the embodiments.
Reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
In the following description, for the purposes of clearly illustrating the structure and operation of the present invention, directional terms are used, but terms such as "front", "rear", "left", "right", "outer", "inner", "outward", "inward", "upper", "lower", etc. should be construed as words of convenience and should not be construed as limiting terms.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
The invention relates to a device and a method for synchronously measuring physical forms and key components of solid particles in a fast pyrolysis process, which mainly have the functions of synchronously measuring and obtaining image signals and product absorption spectrum signals of the solid particles in the fast pyrolysis process, thereby carrying out in-situ analysis on physical and chemical processes of the fast pyrolysis process of the solid particles and carrying out real-time monitoring on transition states and primary products related to the intermediate process.
The invention provides a solid particle measuring device in a pyrolysis process, which is used for measuring the physical form and components of solid particles in the pyrolysis process. The measuring device comprises an absorption cell, photographic equipment, an infrared laser, a lens, a first infrared detector and a second infrared detector. The absorption cell is used for burning a substance to be measured and is provided with a reflecting element, the photographic equipment is matched with the absorption cell and is used for shooting the burning state of the substance, and the infrared laser, the lens, the first infrared light detector and the second infrared light detector are arranged in such a way that infrared light emitted by the infrared laser passes through the lens to form infrared light refraction light and infrared light reflection light, the infrared light reflection light is received by the first infrared light detector, the infrared light refraction light is emitted into the absorption cell, is reflected for multiple times by the reflecting element in the absorption cell, is emitted out of the absorption cell and is received by the second infrared light detector.
The invention can measure the transient combustion process and the release rule of gas-phase products on the millisecond time scale, and meanwhile, the measuring device has the advantages of simple construction, high reliability, rich measuring information, high speed and high accuracy.
As shown in fig. 1, the apparatus for measuring physical form and composition of solid particles in a fast pyrolysis process provided by the present invention includes an infrared laser 1, a first infrared detector 2, an absorption cell 3, a heater 4, a temperature controller 5, a second infrared detector 6, a data acquisition card 7, a computer 8, a photographing device 9, a first reflector 10, a second reflector 11, a third reflector 12, a lens 13, a first cylindrical mirror 14, a second cylindrical mirror 15, a feeding pipe 16, and a quartz window 18. The absorption tank 3 is a cuboid and is used for burning substances to be measured. The infrared laser 1 emits infrared light and forms infrared refracted light and infrared reflected light after passing through the lens 13, the first infrared detector 2 is arranged on a light path of the infrared reflected light after being reflected by the second reflector 11 and receives signals of an absorption spectrum of the infrared reflected light, the first reflector 10 is arranged on a light path of the infrared refracted light after being emitted from the lens 13 and incident into the absorption cell 3, the infrared refracted light enters into the absorption cell 3 after being reflected by the first reflector 10, the first cylindrical mirror 14 and the second cylindrical mirror 15 are symmetrically arranged in the light path direction of the infrared refracted light in the absorption cell 3, the first cylindrical mirror 14 is provided with a light inlet, the second cylindrical mirror 15 is provided with a light outlet, the infrared refracted light enters from the light inlet on the first cylindrical mirror 14 and is emitted from the light outlet on the second cylindrical mirror 15 after being reflected for multiple times on the first cylindrical mirror 14 and the second cylindrical mirror 15, the infrared refracted light passes through the reaction area of the substance to be detected in the absorption cell 3 for multiple times, the third reflector 12 is arranged on the light path of the infrared refracted light emitted from the light outlet of the second cylindrical mirror 15 and leaving the absorption cell 3, and the second infrared detector 6 is arranged on the light path of the infrared refracted light reflected by the third reflector 12. The data acquisition card 7 is connected with the first infrared light detector 2 and the second infrared light detector 6, and the data acquisition card 7 collects the absorption spectrum information collected by the first infrared light detector 2 and the second infrared light detector 6. After the measurement process is finished, the memory card data of the data acquisition card 7 and the camera device 9 can be imported into the computer 8 for data processing and analysis.
As shown in fig. 2, a heater 4 is horizontally disposed at the center of the absorption cell 3, the heater 4 is disposed at the center of the first cylindrical mirror 14 and the second cylindrical mirror 15, the heater 4 is electrically connected to the temperature controller 5, a feeding pipe 16 is vertically disposed above the heater 4, and the substance to be measured enters the absorption cell 3 through the feeding pipe 16 by gravity and falls onto the heater 4. And a quartz window 18 is provided on the side wall of the absorption cell 3, and the photographing device 9 coaxial with the heater 4 and the quartz window 18 is disposed outside the absorption cell 3.
Although the embodiment shown in fig. 1 provides the first reflector 10, the second reflector 11, and the third reflector 12 for changing the propagation direction of the reflected infrared light and the refracted infrared light, it should be understood by those skilled in the art that the present embodiment can also achieve the object of the invention without providing reflectors, for example, the reflected infrared light formed by the infrared light emitted from the infrared laser 1 passing through the lens 13 can be directly received by the first infrared detector 2 without being reflected by the second reflector 11 to obtain the absorption spectrum signal of the reflected infrared light, and the optical path can also be adjusted so that the refracted infrared light formed by the infrared light emitted from the infrared laser 1 passing through the lens 13 can directly enter the absorption cell 3 without being reflected by the first reflector 10, and the refracted infrared light can directly be received by the second infrared detector 6 without being reflected by the third reflector 12 after exiting the absorption cell 3 to obtain the absorbed infrared light A spectral signal. In addition, a plurality of reflecting mirrors can be arranged to adjust the light path to change the propagation direction of the infrared reflected light and/or the infrared refracted light, so that the purpose of reducing the volume of the device or according to actual needs is achieved. The above embodiments do not depart from the content of the present invention.
It is to be understood that the first reflecting mirror 10 is disposed on the entrance optical path of the absorption cell 3 in fig. 1 for the purpose of changing the traveling direction of the infrared light refracted light coming out of the lens 13, the second reflecting mirror 11 is disposed on the entrance optical path of the first infrared light detector 2 for the purpose of changing the traveling direction of the infrared light reflected by the lens 13, and the third reflecting mirror 12 is disposed on the exit optical path of the absorption cell 3 for the purpose of changing the traveling direction of the light coming out of the absorption cell 3, and the disposition of the reflecting mirrors of the present invention is not limited to the embodiment in fig. 1.
In addition, although the absorption cell 3 shown in fig. 1 has a rectangular parallelepiped shape, the shape of the absorption cell 3 is not limited to a rectangular parallelepiped shape, and only a substance to be measured can be burned, and the shape of the absorption cell 3 is not limited to the present invention.
In other embodiments, the first cylindrical mirror 14 and the second cylindrical mirror 15 may not be provided, so that the infrared refracted light enters the absorption cell 3 and leaves the absorption cell 3 after being reflected multiple times on the inner wall of the absorption cell 3, and the number of times of reflection of the infrared refracted light in the same space is increased by providing the first cylindrical mirror 14 and the second cylindrical mirror 15, and those skilled in the art may or may not perform setting according to actual needs without departing from the scope of the present invention. Preferably, the first cylindrical mirror 14 and the second cylindrical mirror 15 are both square cylindrical mirrors with a side length of 50-200mm and a curvature radius of 400mm, and the projections of the reflecting surfaces of the first cylindrical mirror 14 and the second cylindrical mirror 15 are arranged on the same circle.
A heater 4 is provided in the absorption cell 3 for heating the substance to be measured, and alternatively, a silicon carbide heating plate may be used as the heater. The temperature controller 5 is not necessary for the invention, and is used for adjusting the temperature of the heater, the invention only needs to realize the combustion of the substance to be measured, and the heater can be directly closed by the combustion of the substance to be measured without arranging the temperature controller, thereby not departing from the content of the invention. Further, the heater 4 is not essential, and for the purpose of the invention, the substance to be measured is heated to be burned outside the measuring apparatus and then placed in the absorption cell 3. In addition, the heater 4 is not necessarily arranged strictly at the central position of the first cylindrical mirror 14 and the second cylindrical mirror 15, and the heater 4 is arranged only at a position such that the substance to be measured burned placed on the heater 4 can be passed through by the optical path of the infrared light refracted light.
The feed tube 16 is preferably a quartz tube. However, the sample inlet tube 16 is not necessarily provided with a member, and the same function can be achieved by holding the sample to be measured in the absorption cell 3 by other means, for example, with tweezers, without departing from the scope of the present invention.
Fig. 3 is a schematic view of a measuring device according to another embodiment of the present invention. A measuring device according to another embodiment of the present invention is described below with reference to fig. 3. The difference between fig. 3 and the measuring apparatus shown in fig. 1 is that the measuring apparatus shown in fig. 3 further includes a visible light laser 19, a fourth reflector 20, a fifth reflector 21, and a fifth reflector 22, so that the visible light and the infrared light are collimated and coupled, the optical paths of the visible light and the infrared light are overlapped, and the optical paths are adjusted by using the visible light instead of the infrared light. Only the differences between fig. 3 and fig. 1 will be described, and the same reference is made to the related description above, and the details will not be described here.
As shown in fig. 3, a fourth mirror 20 is disposed on the exit optical path of the visible laser 19 for the purpose of changing the propagation direction of the visible light entering the lens 13. The first mirror 10, the fifth mirror 21, the fifth mirror 22 are arranged between the lens 13 and the absorption cell 3 in order to change the direction of propagation of the light from the lens 13 to the absorption cell 3. The light emitted by the visible light laser 19 passes through the lens 13 to form visible light reflected light and visible light refracted light, so that the visible light reflected light is superposed with the infrared light refracted light, and the visible light refracted light is superposed with the infrared light reflected light.
The invention also provides a method for measuring the form and components of solid particles in the pyrolysis process, which comprises the following steps: s1, heating the substance to be measured by using a heater; s2, infrared light is utilized to form infrared light refraction light and infrared light reflection light through a lens, the infrared light reflection light is adjusted to be received by a first infrared light detector, and the infrared light refraction light is adjusted to be received by a second infrared light detector after passing through a reaction area for heating a substance to be measured; and S3, shooting the reaction area by using a shooting device. Preferably, the three steps are performed simultaneously. The method can measure the transient combustion process and the release law of gas-phase products on a millisecond time scale.
In another implementation, the infrared refracted light and the infrared reflected light may also be path-modulated with visible light. The visible light and the infrared light are subjected to collimation coupling, the light path coincidence of the visible light and the infrared light is adjusted, the light can be used for replacing the infrared light to carry out light path debugging, the debugging of the visible light which can be seen by naked eyes is used for replacing the debugging of the infrared light which can not be seen by naked eyes, and the difficulty of light path modulation is reduced. Preferably, visible light is utilized to form visible light refraction light and visible light reflection light after passing through the lens, the visible light refraction light is adjusted to coincide with the infrared light reflection light path, the visible light reflection light is adjusted to coincide with the infrared light refraction light path, and the visible light reflection light is adjusted to reach the second infrared light detector after passing through the reaction area.
In addition, in step S2, a first cylindrical mirror and a second cylindrical mirror may be added, the first cylindrical mirror and the second cylindrical mirror are symmetrically disposed on two sides of the reaction region, and a small hole is respectively disposed on the first cylindrical mirror and the second cylindrical mirror, through which light can pass, and the light path of the infrared refracted light is adjusted so that the infrared refracted light is incident into the reaction region from the small hole of the first cylindrical mirror, and after being reflected between the first cylindrical mirror and the second cylindrical mirror for multiple times, is emitted from the small hole on the second cylindrical mirror, and finally is received by the second infrared detector. Through the arrangement of the first cylindrical mirror and the second cylindrical mirror, the times of infrared refracted light passing through the reaction area are increased, and the signal intensity received by the second infrared light detector is improved.
Further, in step S2, the optical path of the infrared refracted light is adjusted such that the infrared refracted light is reflected at least five times on the first cylindrical mirror and the second cylindrical mirror, respectively, that is, the infrared refracted light passes through the reaction region 10 times, which theoretically can increase the signal received by the second infrared detector by one order of magnitude.
In a specific embodiment, the first cylindrical mirror and the second cylindrical mirror are set to be square cylindrical mirrors with a side length of 50 × 50mm and a curvature radius of 400mm, the square cylindrical mirrors are fixed on two sides of the reaction region, and are divided into two ends located in a circle with a diameter of 800mm, when infrared refracted light enters between the first cylindrical mirror and the second cylindrical mirror, an included angle between the infrared refracted light and a reflection normal of the first reflection needs to be adjusted to be 0.5 °, at this time, the infrared refracted light is reflected 5 times at the first cylindrical mirror and the second cylindrical mirror respectively, that is, the infrared refracted light passes through the reaction region 10 times. Those skilled in the art can adjust the optical path of the infrared refracted light and the specifications of the first cylindrical lens and the second cylindrical lens according to actual needs, and are not limited to the above-mentioned embodiments.
In addition, in step S3, the shutter speed of the image information collected by the camera device is adjusted to be in the range of 1000 and 100000 frames/second. So as to realize the continuous motion track, the ignition process and the phase change process of the substance to be measured in the combustion process.
In addition, in step S2, the frequencies of the infrared light reflected light and the infrared light refracted light collected by the first infrared light detector and the second infrared light detector are adjusted to be within the range of 10000-3000000 Hz. So as to realize microsecond-level time resolution and measure transient change of products in the combustion process.
In one embodiment, in step S1, the substance to be measured is heated by a heater and the heater is adjusted to be heated to a temperature range of 700-. The substance to be measured enters a high-temperature area, phase change can occur after the substance to be measured is heated to reach a melting point, the substance is converted from a solid state to a molten state, some volatile gas phase substances are released, the photographic equipment records the shape change of the substance to be measured in the whole process, and in addition, the volatile gas phase substances start to burn after reaching an ignition point. The temperature of the heater can be adjusted by one skilled in the art according to the properties of the substance to be measured.
In other embodiments, the data acquisition unit may be further used to synchronously collect the absorption spectrum signals acquired by the first infrared light detector and the second infrared light detector.
In addition, 100mL/min of air can be continuously introduced into the reaction area, so that the air atmosphere required by combustion is ensured, and the duration of the combustion process of the substance to be measured is ensured to exceed 3 seconds at least.
FIG. 4 shows measured CO from pyrolysis of corn cobs in an embodiment of the present invention2The release rule and the change process of the physical form of the particles. FIG. 4a shows CO during the combustion of corn cob particles2The release profile, fig. 4b, shows an image of the change in physical form of the corn cob particles during combustion. As shown in the figure, the corncob is heated rapidly by the heat source before 140ms, and the local blackening phenomenon appears on the surface of the particles, so that the sample is subjected to pyrolysis reaction and releases volatile organic compounds to the periphery of the particles. When the temperature of the particle surface is increased to the ignition point of volatile organic compounds by 147ms, an ignition phenomenon occurs, and a more obvious light yellow flame can be seen. Then the flame gradually increased smoothly until the 292ms flame brightness peaked. And then the volatile organic compounds are gradually exhausted, the flame is gradually disappeared to 417ms, the volatile organic compound combustion process is finished, and the combustion time is 277 ms. In the process, the formed coke starts to generate combustion reaction for 1000ms, the combustion time of the corncob coke is 592ms after the combustion is finished. CO detected in this process2The concentration trend of (a) is shown in the graph of fig. 4 a.
The embodiments described above are merely exemplary of the preferred aspects of the present invention, and are not intended to limit the present invention.
The device and the method for measuring the physical form and the key components of the solid particles in the fast pyrolysis process can measure the transient combustion process and the release rule of gas-phase products on a millisecond time scale. The method overcomes the defect that the modulation of the optical path is too complex in the traditional measurement technology, the optical paths of the visible light and the infrared light used for the experiment are superposed by introducing the collimated coupling of the visible light and the infrared light, and the visible light is used for replacing the infrared light to modulate the complex optical path, so that the measurement process is simpler and more accurate. The synchronous measuring device is simple and easy to build, high in reliability, rich in measuring information, high in speed and high in accuracy, and is very suitable for academic research and industrial application.
While the preferred embodiments of the present invention have been illustrated and described in detail, it should be understood that various changes and modifications could be made therein by those skilled in the art after reading the above teachings of the present invention. Such equivalents are intended to fall within the scope of the claims appended hereto.
Claims (20)
1. A solid particle measuring device in the pyrolysis process is used for measuring the physical form and components of solid particles in the pyrolysis process and is characterized by comprising an absorption cell, a photographic device, an infrared laser, a lens, a first infrared detector and a second infrared detector,
the absorption cell is used for burning a substance to be measured and is provided with a reflecting element, and the photographic equipment is matched with the absorption cell and is used for photographing the burning state of the substance;
the infrared laser, the lens, the first infrared light detector and the second infrared light detector are arranged in such a way that infrared light emitted by the infrared laser passes through the lens to form infrared refracted light and infrared reflected light, the infrared reflected light is received by the first infrared light detector, and the infrared refracted light is incident into the absorption cell, reflected by the reflecting element for multiple times in the absorption cell, then emitted out of the absorption cell and received by the second infrared light detector.
2. The measuring device according to claim 1, wherein the measuring device comprises at least one mirror mounted on an optical path of the infrared light reflected light and/or the infrared light refracted light and adapted to change a propagation direction of the infrared light reflected light and/or the infrared light refracted light.
3. The measuring apparatus according to claim 1, wherein the side wall of the absorption cell is provided with at least one see-through window, and the photographing device is installed outside the see-through window and cooperates with the see-through window to photograph the combustion state of the substance in the absorption cell.
4. The measuring apparatus according to claim 1, further comprising a first reflecting mirror disposed on an entrance optical path of the absorption cell and adapted to change a traveling direction of the infrared-light-refracted light exiting from the lens, a second reflecting mirror disposed on an entrance optical path of the first infrared-light detector and adapted to change a traveling direction of the infrared-light-reflected light reflected by the lens, and a third reflecting mirror disposed on an exit optical path of the absorption cell and adapted to change a traveling direction of the light exiting from the absorption cell.
5. The measuring device according to claim 1, wherein the measuring device further comprises a visible light laser, light emitted by the visible light laser forms visible light reflected light and visible light refracted light after passing through the lens, the visible light reflected light is coincident with the infrared light refracted light, and the visible light refracted light is coincident with the infrared light reflected light.
6. The measurement apparatus according to claim 5, further comprising a fourth mirror disposed on an exit optical path of the visible laser and configured to change a propagation direction of the visible light entering the lens, a plurality of fifth mirrors disposed between the lens and the absorption cell and configured to change a propagation direction of the light from the lens to the absorption cell, a sixth mirror disposed on an exit optical path of the absorption cell and configured to change a propagation direction of the light from the absorption cell to the second infrared light detector, and a seventh mirror disposed on an entrance optical path of the first infrared light detector and configured to change a propagation direction of the light reflected by the lens.
7. The measuring device according to claim 1, wherein a first cylindrical mirror and a second cylindrical mirror are disposed in the absorption cell, the first cylindrical mirror and the second cylindrical mirror are disposed opposite to each other in the absorption cell and are respectively located on an inlet optical path and an outlet optical path of the absorption cell, the first cylindrical mirror is provided with a light inlet, the second cylindrical mirror is provided with a light outlet, and light entering the absorption cell after passing through the light inlet exits the absorption cell through the light outlet after being reflected between the first cylindrical mirror and the second cylindrical mirror for multiple times.
In one embodiment, the projections of the reflective surfaces of the first cylindrical mirror and the second cylindrical mirror are arranged on the same circle.
In one embodiment, the first cylindrical mirror and the second cylindrical mirror are both square cylindrical mirrors with the side length between 50mm and 200mm and the curvature radius of 400 mm.
8. The measuring device of claim 1, further comprising a heater disposed within the absorption cell for heating a substance to be measured; preferably, the heater is a silicon carbide heating plate.
In one embodiment, the heater is disposed between the first cylindrical mirror and the second cylindrical mirror, and is preferably disposed at a central position of the first cylindrical mirror and the second cylindrical mirror.
9. The measurement device of claim 8, further comprising a temperature control instrument in circuit with the heater and configured to regulate the temperature of the heater.
10. A measuring device according to claim 1, further comprising a feed tube disposed vertically above the heater, the substance to be measured entering the absorption cell from the feed tube by gravity.
In one embodiment, the feed tube is a quartz tube.
11. The measurement device according to claim 1, further comprising a data acquisition unit in signal connection with the first infrared light detector and the second infrared light detector, respectively, to collect absorption spectrum signals acquired by the first infrared light detector and the second infrared light detector.
In one embodiment, the data acquisition unit is a data acquisition card.
12. The measurement device according to claim 11, further comprising a data processing unit in signal connection with the data acquisition unit and the camera equipment.
In one embodiment, the shutter speed of the photographic device is in the range of 1000 and 100000 frames/second.
In one embodiment, the frequencies of the infrared reflected light and the infrared refracted light collected by the first infrared light detector and the second infrared light detector are in the range of 10000-.
13. A method for measuring the morphology and composition of solid particles in a pyrolysis process, comprising the steps of:
step S1: heating a substance to be measured by using a heater;
step S2: infrared light is utilized to form infrared light refracted light and infrared light reflected light through a lens, the infrared light reflected light is adjusted to be received by a first infrared light detector, and the adjusted infrared light refracted light is adjusted to be received by a second infrared light detector after passing through a reaction area for heating a substance to be measured;
step S3: the reaction area is photographed using a photographing apparatus.
Preferably, the step S1, the step S2 and the step S3 are performed simultaneously.
14. The method of claim 13, further comprising:
step S4: performing light path modulation on the infrared refraction light and the infrared reflection light by using visible light;
preferably, in step S4, visible light is used to form visible light refracted light and visible light reflected light after passing through the lens, the visible light refracted light is adjusted to coincide with the infrared light reflected light optical path, the visible light reflected light is adjusted to coincide with the infrared light refracted light optical path, and the visible light reflected light is adjusted to reach the second infrared light detector after passing through the reaction region.
15. The method according to claim 13, wherein in step S2, a first cylindrical mirror and a second cylindrical mirror are disposed on two opposite sides of the reaction region, and an aperture is disposed on each of the first cylindrical mirror and the second cylindrical mirror, and the optical path of the infrared refracted light is adjusted such that the infrared refracted light enters the reaction region through the aperture on the first cylindrical mirror and is received by the second infrared light detector after being emitted through the aperture on the second cylindrical mirror after being reflected between the first cylindrical mirror and the second cylindrical mirror for a plurality of times.
16. The method according to claim 15, wherein in the step S2, the optical path of the infrared light refracted light is adjusted so that the infrared light refracted light is reflected at least five times on the first cylindrical mirror and the second cylindrical mirror, respectively.
17. The method as claimed in claim 13, wherein in step S3, the shutter speed of the image information captured by the camera device is adjusted to be in the range of 1000 and 100000 frames/sec.
18. The method as claimed in claim 13, wherein in step S2, the frequencies of the infrared reflected light and the infrared refracted light collected by the first infrared light detector and the second infrared light detector are adjusted to be within the range of 10000-3000000 Hz.
19. The method as claimed in claim 13, wherein in step S1, the substance to be measured is heated by a heater, and the heater is adjusted to a temperature range of 700-1200K before the substance to be measured is heated.
20. The method of claim 13, further comprising collecting the absorption spectrum signals collected by the first infrared light detector and the second infrared light detector simultaneously with a data collection unit.
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