CN112415039B - Free radical in-situ online detection device in high-temperature conversion process of organic materials - Google Patents
Free radical in-situ online detection device in high-temperature conversion process of organic materials Download PDFInfo
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Abstract
An in-situ online detection device for free radicals in the high-temperature conversion process of organic materials comprises a free radical detection module, a reaction tank, a temperature control module, a displacement detection and regulation module, a reaction gas control module and a computer control module; the free radical detection module comprises an electron paramagnetic resonance spectrometer, and a light source channel is arranged in the electron paramagnetic resonance spectrometer; the reaction tank is placed in an electron paramagnetic resonance spectrometer and consists of three layers of quartz tubes, wherein the central layer is a material reaction region, and the outer parts of the reaction tank are respectively a vacuum heat insulation layer and a forced heat dissipation layer; the temperature control module comprises a laser emission unit and an infrared temperature measurement unit and is used for irradiating reaction materials and measuring temperature; the displacement detection and regulation module detects the offset of the laser emission unit and adjusts the positions of the laser emission unit and the infrared temperature measurement unit; the reaction gas control module supplies gas into the reaction tank. The invention can realize that when the sample reacts at the temperature of more than 1000 ℃, the temperature of the electron paramagnetic resonance spectrometer is lower than 40 ℃, and the detection is ensured to be continuously and smoothly carried out.
Description
Technical Field
The invention relates to a free radical detection device, in particular to an in-situ online detection device for free radicals in a high-temperature conversion process of organic materials.
Background
Organic materials, such as coal, petroleum and small molecule methanol, furfural and the like, undergo a radical reaction as a main chemical reaction body in a high-temperature conversion process. When designing a high-efficiency conversion reactor for various organic materials, the reaction mechanism of the organic materials needs to be understood deeply, and a targeted reactor structure is designed based on the accurate description of the reaction mechanism, so that the material reaction conversion rate is improved to the maximum extent, side reactions are inhibited, and the overall efficiency of the system is improved.
At present, research and development personnel rarely relate to the research on the free radical reaction process when researching the reaction mechanism of the organic material, and mainly deduce the reaction generated in the reaction process based on the characterization analysis of the reaction product so as to determine the reaction mechanism. The method lacks the description of the most critical free radical reaction mechanism in the reaction process, so the obtained reaction mechanism is inaccurate and is difficult to correctly guide the design of a high-efficiency reactor.
In recent years, researchers have recognized the importance of radical reactions in the high temperature conversion of organic materials, and have therefore begun to explore the reaction mechanism of organic materials in depth from the perspective of radical reactions to guide reactor development. The free radicals can be detected by using an electron paramagnetic resonance spectrometer, but because more than 99.9 percent of the free radicals rapidly react in the reaction process and are converted into more stable non-free radical substances, the free radical reaction mechanism cannot be correctly described by analyzing the free radical information in the product by a non-in-situ detection method, and the free radicals participating in the reaction process must be characterized by an in-situ online detection means.
The main technical difficulty of the high-temperature in-situ on-line detection of the free radicals is that the magnet of the electron paramagnetic resonance spectrometer cannot resist high temperature, and the test effect is very poor when the temperature of the magnet is higher than 40 ℃. However, when the high-temperature in-situ online detection is performed, the sample is located at the center of the resonant cavity, and the reaction time is usually long (the reaction process is long), so that the heat of the sample and the high-temperature region around the sample is conducted to the magnet, and finally the temperature of the magnet of the electron paramagnetic resonance spectrometer is increased, so that the test cannot be performed smoothly. In addition, the resonant cavity space of the electron paramagnetic resonance spectrometer is small, and a sample heating device and a heat dissipation module are difficult to arrange, so that the high-temperature in-situ online detection function of the free radicals is difficult to expand. Therefore, it is necessary to adopt advanced technical means for the electron paramagnetic resonance spectrometer to realize the high-temperature in-situ online detection function of the free radicals.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention aims to provide a free radical in-situ online detection device in the high-temperature organic material conversion process, so as to solve the problem that the in-situ free radical online detection in the high-temperature organic material conversion process by using an electron paramagnetic resonance spectrometer is difficult to realize in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an in-situ on-line detection device for free radicals in the high-temperature conversion process of organic materials comprises a free radical detection module, a reaction tank, a temperature control module, a displacement detection and regulation module, a reaction gas control module and a computer control module; wherein,
the free radical detection module comprises an electron paramagnetic resonance spectrometer, and a light source channel is arranged at the center of the electron paramagnetic resonance spectrometer;
the reaction tank is formed by sleeving three quartz tubes, the central layer of the reaction tank is a material reaction area for placing a sample to be detected, the outer layer of the central layer is a vacuum heat insulation layer, the outer layer of the vacuum heat insulation layer is a forced heat dissipation layer, and the reaction tank is placed in an electron paramagnetic resonance spectrometer and is vertical to the light source channel;
the temperature control module comprises a laser emission unit and an infrared temperature measurement unit, the laser emission unit is positioned at one end of the electron paramagnetic resonance spectrometer and corresponds to the light source channel, the infrared temperature measurement unit is positioned at the other end of the electron paramagnetic resonance spectrometer and corresponds to the light source channel, the laser emission unit emits laser to irradiate and heat a sample to be measured in the reaction tank through the light source channel, and the infrared temperature measurement unit performs non-contact temperature measurement on the sample to be measured;
the displacement detection and regulation module comprises a stepping motor and a lifting cradle head, the two lifting cradle heads are respectively positioned at two ends of an electron paramagnetic resonance spectrometer, the height of the lifting cradle head is controlled by the stepping motor, and the laser emission unit and the infrared temperature measurement unit are respectively positioned on the lifting cradle head;
the reaction gas control module comprises a gas source and a mass flow meter, the gas source is connected with the reaction tank through a pipeline, and the mass flow meter is installed on the pipeline;
the computer control module is used for controlling the laser emission unit, the electron paramagnetic resonance spectrometer, the reaction gas control module and the displacement detection and regulation module to realize the cooperative work among different modules.
Preferably, the laser emission unit generates laser with light source wavelength of 1064nm, 980nm and 808nm, the beam diameter of the laser is not more than 5nm, and the power of the laser emission unit is adjusted by the computer control module.
Preferably, the laser emitting unit is provided with a beam collimator to adjust a beam diameter of the laser.
Furthermore, a graphite ring is arranged on one side of the laser emission unit corresponding to the electron paramagnetic resonance spectrometer, and the graphite ring absorbs the offset laser energy.
Furthermore, a thermocouple temperature measuring unit is arranged in the graphite ring and used for detecting the temperature rising position of the graphite ring and feeding the temperature rising position back to the computer control module, the offset position of the laser emission unit is determined through the computer control module, an offset position signal is transmitted to the displacement monitoring and regulating module, and the lifting cradle head is regulated and controlled through the stepping motor, so that the laser emission unit and the infrared temperature measuring unit are regulated to correct positions.
Furthermore, both ends of the vacuum heat insulation layer are of a closed structure or one end of the vacuum heat insulation layer is of a through structure and the other end of the vacuum heat insulation layer is of a closed structure, and when one end of the vacuum heat insulation layer is of a through structure and the other end of the vacuum heat insulation layer is of a closed structure, the through end is connected with a vacuum pump to maintain the vacuum degree in the vacuum heat insulation layer.
Furthermore, two ends of the forced heat dissipation layer are of a through structure, and cooling gas or cooling liquid is introduced into the through structure to realize forced heat dissipation.
Furthermore, the gas source in the reaction gas control module is a high-pressure gas cylinder which is respectively filled with cooling gas and reaction gas, wherein the reaction gas is introduced into the material reaction zone, the cooling gas is introduced into the forced heat dissipation layer, and a reaction gas preheating device is arranged on a pipeline of the reaction gas.
Preferably, the reaction gas preheating device is a temperature-controllable resistance furnace.
The invention has the beneficial effects that:
the method meets the requirement of in-situ free radical on-line detection in the material reaction process under the high-temperature condition, and fills the blank of the high-temperature in-situ free radical on-line detection. The laser serves as an external heat source, temperature feedback control is carried out by matching infrared temperature measurement, and accurate heating and temperature control of materials can be achieved. The three-layer quartz tube reaction tank can prevent heat generated by sample reaction from being conducted to the electron paramagnetic resonance spectrometer, and the overtemperature of a magnet of the electron paramagnetic resonance spectrometer is avoided to the maximum extent. By combining the structure, the temperature of the electron paramagnetic resonance spectrometer is lower than 40 ℃ when the sample reacts at the temperature of more than 1000 ℃, and the continuous and smooth detection is ensured.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of a reaction gas preheating apparatus according to the present invention;
FIG. 3 is a schematic view of the structure of a reaction tank according to the present invention;
FIG. 4 is a schematic view of a partial structure of a reaction tank according to the present invention;
in the figure: the device comprises a laser emission unit 1, a beam collimator 1.1, an infrared temperature measurement unit 2, an electron paramagnetic resonance spectrometer 3.1 graphite ring, a reaction gas control module 4, a mass flow meter 4.1, a reaction gas preheating device 4.2, a computer control module 5, a lifting cradle head 6, a reaction tank 7, a material reaction area 7.1, a vacuum thermal insulation layer 7.2 and a forced heat dissipation layer 7.3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Referring to fig. 1, an in-situ on-line detection device for free radicals in the high-temperature conversion process of organic materials comprises a free radical detection module, a reaction tank 7, a temperature control module, a displacement detection and regulation module, a reaction gas control module 4 and a computer control module 5.
The free radical detection module comprises an electron paramagnetic resonance spectrometer 3, and a light source channel is arranged in the center of the electron paramagnetic resonance spectrometer 3; the time resolution of the electron paramagnetic resonance spectrometer 3 is less than 0.001s, and the magnetic field range is as follows: 0-650mT, the magnet has the forced air cooling or water cooling function, which is convenient for the instrument to dissipate heat and ensures the normal detection. The electron paramagnetic resonance spectrometer 3 has the function of detecting the temperature of a magnet, when the instrument is over-temperature, the laser light source is closed through a computer, and the free radical detection module is connected with the computer control module 5 through a data line.
Referring to fig. 3 and 4, the reaction tank 7 is formed by sleeving three quartz tubes, and the central layer is a material reaction area 7.1 for placing a sample to be measured, preferably, the diameter of the central layer is 5mm, and two ends of the central layer are through and provided with connectors for connecting with pipelines of reaction gas and cooling gas. The outer layer of the central layer is a vacuum heat insulation layer 7.2, two ends of the vacuum heat insulation layer 7.2 are of closed structures or one end of the vacuum heat insulation layer is of a through structure, the other end of the vacuum heat insulation layer is of a closed structure, when the two ends of the vacuum heat insulation layer are of closed structures, the interior of the vacuum heat insulation layer is vacuumized in advance, and when one end of the vacuum heat insulation layer is of a through structure and the other end of the vacuum heat insulation layer is of a closed structure, the through end is connected with a vacuum pump to maintain the vacuum degree in the vacuum heat insulation layer 7.2. The outer layer of the vacuum heat insulation layer 7.2 is a forced heat dissipation layer 7.3, two ends of the forced heat dissipation layer 7.3 are of a through structure, and cooling gas or cooling liquid is introduced into the through structure to realize forced heat dissipation of the whole reaction tank 7. The reaction tank 7 is arranged at the center of the electron paramagnetic resonance spectrometer 3 and is vertical to the light source channel.
Referring to fig. 1 again, the temperature control module includes a laser emission unit 1 and an infrared temperature measurement unit 2, the laser emission unit 1 is located at one end of the electron paramagnetic resonance spectrometer 3 and corresponds to the light source channel, preferably, the laser emission unit 1 generates laser with light source wavelength of 1064nm, 980nm, 808nm, the beam diameter of the laser is not more than 5nm, preferably, the laser emission unit 1 is equipped with a beam collimator 1.1 for adjusting the beam diameter of the laser, and the energy attenuation of the laser emitted by the laser emission unit 1 is less than 1% within 1 meter from the light source; the power of the laser emission unit 1 can be controlled by a computer and flexibly adjusted; the laser emission unit 1 is placed at a position where laser light is vertically injected into an electron paramagnetic resonance spectrometer 3; the laser emitting unit 1 is connected with a computer control module 5 through a data line.
The infrared temperature measuring unit 2 is positioned at the other end of the electron paramagnetic resonance spectrometer 3 and corresponds to the light source channel, the non-contact detection can be carried out on the temperature of the material, the response time is less than 0.1s, and the infrared temperature measuring unit 2 adopts the prior art means; as shown in fig. 1, a circle of graphite ring 3.1 is arranged around the light source channel at the outer side of the laser emission unit 1 corresponding to the electron paramagnetic resonance spectrometer 3, so as to absorb the laser energy passing through the electron paramagnetic resonance spectrometer 3 due to the offset; there is thermocouple temperature measurement unit under graphite circle 3.1, thermocouple temperature measurement unit can detect the change of graphite circle 3.1 temperature everywhere, when laser emission unit 1 takes place the skew, laser can't pass through light source passageway and shine reaction tank 7, laser can shine on graphite circle 3.1 this moment, and then arouse graphite circle 3.1 local intensification, thermocouple temperature measurement unit detects the position of local intensification and with signal transmission to computer control module 5, computer control module 5 can transmit the step motor of signal to laser emission unit 1 department this moment, adjust laser emission unit 1's position through the position of step motor control lift cloud platform 6, make laser shine reaction tank 7 through the light source passageway smoothly. The infrared temperature measuring unit 2 and the laser emitting unit 1 are symmetrically arranged at two ends of the electron paramagnetic resonance spectrometer 3. The laser emission unit 1 emits laser to irradiate and heat a sample to be measured in the reaction tank 7 through a light source channel, and the infrared temperature measurement unit 2 performs non-contact temperature measurement on the sample to be measured;
the displacement detection and regulation module comprises a stepping motor and a lifting cloud platform 6, the stepping motor and the lifting cloud platform 6 are respectively arranged at two ends of an electron paramagnetic resonance spectrometer 3, the stepping motor controls the lifting cloud platform 6 to move up and down, the laser emission unit 1 and the infrared temperature measurement unit 2 are respectively arranged on the lifting cloud platform 6, and the movement of the stepping motor is controlled by the computer control module 5 so as to control the lifting cloud platform 6 to move to achieve the purpose of adjusting the positions of the laser emission unit 1 and the infrared temperature measurement unit 2.
The reaction gas control module 4 comprises a gas source and a mass flow meter 4.1, preferably, the gas source is a high-pressure gas cylinder, at least two of the high-pressure gas cylinders are respectively filled with cooling gas and reaction gas, wherein the high-pressure gas cylinder of the reaction gas is connected with the central layer of the reaction tank 7 through a pipeline, preferably, the reaction gas comprises nitrogen, oxygen, carbon dioxide and water vapor, the high-pressure gas cylinder of the cooling gas is connected with a forced heat dissipation layer of the reaction tank through a pipeline, the cooling gas is preferably compressed air, and it should be understood that the high-pressure gas cylinder filled with the cooling gas can also be replaced by a device for providing cooling liquid, the device is connected with the forced heat dissipation layer, and the cooling liquid is introduced into the forced heat dissipation layer for cooling. A reaction gas preheating device 4.2 is arranged on the reaction gas pipeline, preferably, the reaction gas preheating device 4.2 is a temperature-controllable resistance furnace, and is connected with the computer control module 5, and the temperature is adjusted through the computer control module 5. Mass flow meter 4.1 installs respectively on reaction gas light and cooling gas pipeline and all links to each other with computer control module 5, controls gas flow through mass flow meter 4.1.
The computer control module 5 is used for controlling the laser emission unit 1, the electron paramagnetic resonance spectrometer 3, the reaction gas control module 4, and the displacement detection and regulation module to realize cooperative work among different modules, and it should be understood that the operation by the computer control device is a prior art means, and a detailed description is not provided herein.
Further, the organic material in the present invention is an organic material containing a covalent bond structure, and the high temperature bond breaking generates a radical, which includes, but is not limited to: coal, petroleum, biomass, plastics.
Further, the high temperature conversion process in the present invention is a thermal conversion reaction, which includes, but is not limited to: pyrolysis, combustion, gasification and catalytic conversion reaction.
It should be understood that the above description of the preferred embodiments is given for clarity and not for any purpose of limitation, and that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The utility model provides a free radical in situ on-line measuring device among organic material high temperature conversion process which characterized in that: the device comprises a free radical detection module, a reaction tank, a temperature control module, a displacement detection and regulation module, a reaction gas control module and a computer control module; wherein,
the free radical detection module comprises an electron paramagnetic resonance spectrometer, and a light source channel is arranged at the center of the electron paramagnetic resonance spectrometer;
the reaction tank is formed by sleeving three quartz tubes, the central layer of the reaction tank is a material reaction area for placing a sample to be detected, the outer layer of the central layer is a vacuum heat insulation layer, the outer layer of the vacuum heat insulation layer is a forced heat dissipation layer, and the reaction tank is placed in an electron paramagnetic resonance spectrometer and is vertical to the light source channel;
the temperature control module comprises a laser emission unit and an infrared temperature measurement unit, the laser emission unit is positioned at one end of the electron paramagnetic resonance spectrometer and corresponds to the light source channel, the infrared temperature measurement unit is positioned at the other end of the electron paramagnetic resonance spectrometer and corresponds to the light source channel, the laser emission unit emits laser to irradiate and heat a sample to be measured in the reaction tank through the light source channel, and the infrared temperature measurement unit performs non-contact temperature measurement on the sample to be measured;
the displacement detection and regulation module comprises a stepping motor and a lifting cradle head, the two lifting cradle heads are respectively positioned at two ends of an electron paramagnetic resonance spectrometer, the height of the lifting cradle head is controlled by the stepping motor, and the laser emission unit and the infrared temperature measurement unit are respectively positioned on the lifting cradle head;
the reaction gas control module comprises a gas source and a mass flow meter, the gas source is respectively connected with two ends of the reaction tank through pipelines, and the mass flow meter is arranged on the pipelines;
the computer control module is used for controlling the laser emission unit, the electron paramagnetic resonance spectrometer, the reaction gas control module and the displacement detection and regulation module to realize the cooperative work among different modules;
a graphite ring is arranged on one side of the laser emission unit corresponding to the electron paramagnetic resonance spectrometer, and the graphite ring absorbs the offset laser energy;
the graphite ring is internally provided with a thermocouple temperature measuring unit for detecting the temperature rising position of the graphite ring and feeding back the temperature rising position to the computer control module, the offset position of the laser emission unit is determined by the computer control module, an offset position signal is transmitted to the displacement monitoring and regulating module, and the lifting cradle head is regulated and controlled by the stepping motor, so that the laser emission unit and the infrared temperature measuring unit are regulated to correct positions.
2. The device for detecting the in-situ free radicals in the high-temperature organic material conversion process according to claim 1, wherein: the laser emission unit generates lasers with light source wavelengths of 1064nm, 980nm and 808nm, the beam diameter of the lasers is not more than 5nm, and the power of the laser emission unit is adjusted by the computer control module.
3. The device for detecting the in-situ free radicals in the high-temperature organic material conversion process according to claim 2, wherein: the laser emitting unit is provided with a beam collimator for adjusting a beam diameter of the laser.
4. The device for detecting the in-situ free radicals in the high-temperature organic material conversion process according to claim 1, wherein: the vacuum heat insulation layer is characterized in that two ends of the vacuum heat insulation layer are of closed structures or one end of the vacuum heat insulation layer is of a through structure and the other end of the vacuum heat insulation layer is of a closed structure, and when one end of the vacuum heat insulation layer is of a through structure and the other end of the vacuum heat insulation layer is of a closed structure, the through end is connected with a vacuum pump to maintain the vacuum degree in the vacuum heat insulation layer.
5. The device for detecting the in-situ free radicals in the high-temperature organic material conversion process according to claim 1, wherein: two ends of the forced heat dissipation layer are of through structures, and cooling gas or cooling liquid is introduced into the through structures to realize forced heat dissipation.
6. The device for detecting the in-situ free radicals in the high-temperature organic material conversion process according to claim 5, wherein: the gas source in the reaction gas control module is a high-pressure gas cylinder and is respectively filled with cooling gas and reaction gas, wherein the reaction gas is introduced into the material reaction zone, the cooling gas is introduced into the forced heat dissipation layer, and a reaction gas preheating device is arranged on a pipeline of the reaction gas.
7. The device for detecting the in-situ free radicals in the high-temperature organic material conversion process according to claim 6, wherein: the reaction gas preheating device is a temperature-controllable resistance furnace.
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| CN108956360A (en) * | 2018-04-11 | 2018-12-07 | 华中科技大学 | The magnetic suspension thermobalance being rapidly heated based on photo-thermal |
| CN110988009A (en) * | 2019-11-22 | 2020-04-10 | 浙江大学 | Pyrolysis reaction resonant cavity and EPR spectrometer |
| CN111398330A (en) * | 2020-03-18 | 2020-07-10 | 南京大学 | In-situ electron paramagnetic resonance test reaction device and test method thereof |
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