CN112710697A - High-controllable high-stability automatic sample introduction type photo-thermal catalytic reactor and testing method - Google Patents
High-controllable high-stability automatic sample introduction type photo-thermal catalytic reactor and testing method Download PDFInfo
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- CN112710697A CN112710697A CN202011545067.5A CN202011545067A CN112710697A CN 112710697 A CN112710697 A CN 112710697A CN 202011545067 A CN202011545067 A CN 202011545067A CN 112710697 A CN112710697 A CN 112710697A
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 24
- 238000012360 testing method Methods 0.000 title claims description 32
- 239000007789 gas Substances 0.000 claims abstract description 106
- 238000006243 chemical reaction Methods 0.000 claims abstract description 67
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 38
- 230000003287 optical effect Effects 0.000 claims abstract description 32
- 239000012495 reaction gas Substances 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 230000005284 excitation Effects 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims description 15
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 14
- 238000006555 catalytic reaction Methods 0.000 claims description 13
- 238000009529 body temperature measurement Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 4
- 238000010998 test method Methods 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- 238000002347 injection Methods 0.000 description 11
- 239000007924 injection Substances 0.000 description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000004861 thermometry Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
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- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
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- 238000006731 degradation reaction Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/24—Automatic injection systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The invention discloses a high-controllable high-stability automatic sample introduction type photothermal catalytic reactor, which comprises a cover plate, a reaction cavity and a sample table, wherein the cover plate is covered on the top of the reaction cavity; the cover plate comprises an upper cover plate and a lower cover plate, wherein two corresponding optical windows are arranged on the upper cover plate, and a temperature measuring port of the thermal infrared imager is aligned to one of the optical windows; the excitation light source is aligned with the other optical window; the side wall of the reaction cavity is provided with an air inlet, an air outlet and an air outlet, wherein the air inlet is connected with an air cylinder, the air outlet is connected with a peristaltic pump, reaction gas is pumped out from the air outlet through the peristaltic pump and then is introduced into a gas chromatograph for detection, and redundant gas is discharged into the reaction cavity from the air inlet through a pipeline; the exhaust port is used for exhausting residual gas in the reaction cavity and is used as an access port of the thermocouple wire; and a thermocouple clamp is arranged on the sample table and used for fixing a thermocouple placed from the exhaust port.
Description
Technical Field
The invention relates to the field of gas catalytic quantitative determination, in particular to a high-controllable high-stability automatic sample injection type photo-thermal catalytic reactor and a testing method.
Background
Many materials have a thermocatalytic effect, and are widely used for organic synthesis, pollutant degradation and clean energy production by people. It was also found that these reactions can also occur under light excitation. The photocatalytic reaction has the advantages of mild reaction conditions, small secondary pollution, low operation cost, hopeful use of sunlight as a reaction light source and the like. The photothermal effect due to light exposure causes the temperature of the material to rise, and also contributes to the increase in the rate of catalytic reaction. In recent years, the catalytic effect of materials under the combined action of light and heat has attracted much attention.
In principle, light irradiation produces two mechanisms of action, non-thermal and photothermal. Accurate measurement of temperature changes on the surface of a sample caused by light irradiation is important for determining the photothermal reaction mechanism. Accurate determination of the sample temperature depends on the measurement method, and one usually places a thermocouple on the bottom or surface of the sample to measure the temperature, which has large error. Due to the fact that the temperature field is not uniform caused by the photo-thermal effect, temperature gradients can be formed among the surface of the sample, the thermocouple and the environment, and the temperature measured by the thermocouple cannot reflect the real temperature of the surface of the sample. Usually, the different light intensity distributions of the exciting light can cause different photothermal effects at different parts of the surface of the sample, so that the temperature distribution of the surface of the sample is not uniform, and the temperature distribution of the whole illumination surface is difficult to accurately detect by the single-point temperature measurement of the tip of the thermocouple. The contribution to the photothermal effect can be accurately evaluated by measuring the average temperature of the entire illuminated surface using a non-contact method, thereby determining the photothermal catalytic mechanism.
In addition, many simple catalytic reactors operate using syringe pumping, injection sampling, which makes the experiment unstable and increases the workload of the experimenters. Some gas chromatographs are equipped with an automatic sample injection valve but do not have a sample injection pump, and need an external gas pump. These pumps generally operate continuously during the test period, and the test gas increases the possibility of gas leakage of the reaction apparatus during continuous circulation, and also increases the instability of the test, thereby reducing the repeatability and reliability of the test data. The continuous operation of the gas pump also results in a reduced pump life, and if a peristaltic pump is used, the special pump tube may need to be replaced frequently, which increases the testing cost.
Therefore, in the photo-thermal catalysis test, a reactor which can realize high-precision measurement of the surface temperature of the sample, stable and controllable gas measurement process and automatic sample introduction is still lacked.
Disclosure of Invention
The invention aims to provide a low-cost reactor which is convenient to install, can be well matched with a gas chromatograph with an automatic sample injection valve control, can accurately measure the average temperature of the surface of a sample after illumination, and can realize stable and controllable sample injection detection.
The technical scheme adopted by the invention is as follows:
the high-controllable high-stability automatic sample introduction type photothermal catalytic reactor comprises a cover plate, a reaction cavity and a sample table, wherein the cover plate is covered on the top of the reaction cavity, and the sample table is arranged in the reaction cavity;
the cover plate comprises an upper cover plate and a lower cover plate, two optical windows are arranged on the upper cover plate, and a temperature measuring port of the thermal infrared imager is aligned to one of the optical windows; the excitation light source is aligned with the other optical window;
the side wall of the reaction cavity is provided with an air inlet, an air outlet and an air outlet, wherein the air inlet is connected with an air cylinder, the air outlet is connected with a peristaltic pump, the peristaltic pump is connected with a gas chromatograph through a conduit, and the air inlet is also connected with the gas chromatograph through a pipeline; the exhaust port is used for exhausting residual gas in the reaction cavity and is used as an access port of the thermocouple wire;
and a thermocouple clamp is arranged on the sample table and used for fixing a thermocouple placed from the exhaust port.
According to the technical scheme, the two optical windows are made of quartz glass and potassium bromide sheets, and are fixed on the cover plate in a sealing mode through O-shaped rubber rings.
According to the technical scheme, a hole is reserved in the center of the sample table, and a groove is formed in the bottom of the sample table and used for assembling a thermocouple to test the temperature of the backlight area on the bottom surface of the sample.
According to the technical scheme, the reaction cavity is made of glass, the sample table, the thermocouple clamp and the lower cover plate are made of aluminum alloy materials, and the upper cover plate is made of resin materials.
In connection with the above technical scheme, the upper cover plate and the lower cover plate are tightly fixed on the reaction chamber through screws.
According to the technical scheme, the upper cover plate and the lower cover plate are both provided with grooves for fixing the quartz glass sheet and the potassium bromide sheet.
According to the technical scheme, the exhaust port of the reaction cavity is connected with the waste gas treatment device through a pipeline.
The invention also provides a high-controllable high-stability automatic sample introduction type photo-thermal catalytic reaction testing device, which comprises the high-controllable high-stability automatic sample introduction type photo-thermal catalytic reactor, a light source for excitation, an infrared temperature measurement module and an atmosphere circulating system;
the infrared temperature measuring module comprises a thermocouple, an infrared thermal imager and a heating plate, and the heating plate is arranged below the reaction cavity and used for heating the reaction cavity; the thermocouple is fixed on the surface of the sample through the exhaust port; a temperature measuring port of the thermal infrared imager aligns to one of the optical windows to carry out infrared temperature measurement; the excitation light source is aligned to the other optical window to irradiate the surface of the sample;
the atmosphere circulating system comprises a peristaltic pump, a gas chromatograph, a time control switch, a gas cylinder and a flow controller, wherein the peristaltic pump is connected with a gas outlet and the gas chromatograph through a pipeline; the time control switch is connected with the peristaltic pump and is used for controlling the peristaltic pump to be turned on and off at regular time; the flow controller is connected with the gas cylinder and the gas inlet through the gas guide pipe, reaction gas in the gas cylinder enters the reaction cavity from the gas inlet through the flow controller, the reaction gas is pumped out from the gas outlet through the peristaltic pump and then is guided into the gas chromatograph for detection, and redundant gas is discharged into the reaction cavity from the gas inlet through the pipeline.
The invention also provides a high-controllable high-stability automatic sample introduction type photo-thermal catalytic reaction testing method, which is based on the technical scheme and specifically comprises the following steps:
(1) preparing a sample to be tested according to the size of the sample table;
(2) placing a sample to be tested into a sample groove in a sample table, placing the sample table into a reaction cavity, fixing the tip of a temperature thermocouple on the surface of the sample through an exhaust port, extending a thermocouple lead out of the reaction cavity, and fixing a cover plate on the reaction cavity;
(3) connecting the gas outlet with a peristaltic pump, pumping out the reaction gas from the gas outlet through the peristaltic pump, introducing the reaction gas into a gas chromatograph for detection, and discharging the redundant gas into the reaction cavity from the gas inlet through a pipeline; discharging residual gas in the reaction chamber from an exhaust port;
(3) adjusting the surface temperature of the sample to a required temperature and stabilizing the surface temperature in a dark state, introducing reaction gas to be detected into the reaction cavity through the gas inlet, and detecting the surface temperature of the sample through one optical window by using a thermal infrared imager after the concentration of the gas in the reaction cavity is stabilized;
(4) starting exciting light, directly irradiating the surface of the sample through another optical window, simultaneously detecting the change of the surface temperature of the sample under the irradiation of the light by using a thermocouple and a thermal infrared imager, and starting a gas chromatograph for automatic cycle test after the surface temperature is stable.
In connection with the above technical solution, the method further comprises the steps of:
(5) and after the test is finished, closing the gas chromatograph, the thermocouple and the peristaltic pump, taking out the sample on the sample table, and cleaning the sample table.
The invention has the following beneficial effects: the high-precision high-stability automatic sample injection type photo-thermal catalytic reactor can be used for accurately detecting the photo-thermal catalytic reaction of gas phase. The external thermal infrared imager can directly penetrate through the optical window to test the temperature distribution and the average temperature of the surface of the sample in photo-thermal catalysis, and the thermocouple is also arranged on the surface of the sample, so that the difference between two temperature measurement modes can be visually contrasted, and the photo-thermal reaction mechanism can be deeply researched. In addition, a closed internal circulation system is adopted, so that the gas consumption is greatly reduced while high-stability detection is ensured, and the test cost is reduced.
Furthermore, the testing stability and accuracy are greatly improved by controlling the matching work of the peristaltic pump and the gas chromatograph through the time control switch, and the service life of the peristaltic pump (comprising a pump head, a motor and a hose) can be prolonged.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is an overall model view of a photothermal catalytic reactor according to an embodiment of the present invention;
FIG. 2 is a perspective view of the cover plate;
FIG. 3 is a block diagram of a reaction chamber;
FIG. 4 is a structural view of a sample stage;
FIG. 5 is a schematic diagram of an optical path, an atmosphere flow path, and a temperature control and measurement in accordance with an embodiment of the present invention;
FIG. 6 is a graph of gas concentration versus time for P25 catalyzed isopropanol to acetone in the reactor for the GC test;
FIG. 7(a) is an atmosphere product detection diagram with autonomous sample injection using a time controlled switch;
FIG. 7(b) is a diagram of atmospheric product detection without a time switch;
FIG. 8 is a graph of converted acetone product concentration versus gas source standard gas for the gas source peak area of FIG. 7 (a);
FIG. 9(a) is an infrared thermometry of a sample before illumination;
FIG. 9(b) is an infrared thermometry chart of the sample in the light receiving area after the lamp is turned on;
FIG. 9(c) is an infrared thermometry chart of a sample that is not in the light zone after the lamp is turned on;
FIG. 10(a) is a graph of thermocouple thermometry of a sample before illumination;
FIG. 10(b) is a graph of thermocouple thermometry of the sample 10min after lamp-on.
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.
Example 1
The invention provides a high-precision high-stability automatic sample-feeding type photo-thermal catalytic reactor, wherein a catalyst is filled in the reactor and reaction gas is introduced into the reactor, a gas chromatograph is used for testing the concentration of the reaction gas, a thermocouple and an infrared thermal imager are used for testing the surface temperature of a sample in the catalytic process, and a time control switch and a peristaltic pump are used for realizing the controllable injection and circulation of the reaction gas. Wherein the reactor is the main part of the present invention. Fig. 1 is an assembly view of a reactor for photothermal catalysis according to the present invention, which includes a cover plate 1, a reaction chamber 2, and a sample stage 3 inside thereof.
Fig. 2 is a split view of the cover plate 1 of the present invention, which is composed of an upper cover plate 11 and a lower cover plate 12, and two optical windows in the middle, wherein two optical sheets, namely a quartz glass sheet 13 and a potassium bromide sheet 14, are embedded in the two optical windows of the present invention. The three parts can be tightly connected by a hexagonal screw 15 passing through a threaded port of the cover plate to extrude the O-shaped fluorine rubber ring 16. Both cover plates are left with grooves 111, 112, 121, and 122 to fix the optical window sheets. The models of the upper cover plate 11 and the lower cover plate 12 are the same, and the reserved screw can be matched with a hexagonal screw of M6 model.
Fig. 3 is a schematic view of a reaction chamber, the side wall of which is provided with three ports 21, 22 and 23. The reaction gas is pumped out from the gas outlet 23 by a peristaltic pump and is guided into the gas chromatograph for detection, and the redundant gas is discharged into the reaction cavity from the gas inlet 21 through a pipeline. Exhaust port 22 may be used as a reaction chamber residual gas exhaust port and also as an inlet port for a thermocouple wire. The threaded port 24 of M6 is used for connecting the screw of M6 x 30 with the cover plate.
Fig. 4 is a schematic diagram of the sample stage 3, the sample stage 3 is provided with a thermocouple clamp 31 which can cooperate with a U-shaped lock of model M3 to fix a thermocouple, a sample groove 33 is reserved for fixing a sample, and a central hole 32 and a bottom arc-shaped groove 34 can be used for passing through the thermocouple to measure the temperature of a sample bottom backlight area.
FIG. 5 is a schematic diagram of a highly controllable and highly stable auto-sampling type photo-thermal catalytic reaction testing device, which comprises an excitation light source, an infrared temperature measurement module, an atmosphere circulating system and a reactor.
The reactor is essentially the reactor of the embodiment of figure 1.
The infrared temperature measuring module mainly comprises a thermocouple, a thermal infrared imager and a heating plate. The heating plate is arranged below the reaction cavity and heats the reaction cavity. The thermocouple is fixed on the surface of the sample through the exhaust port; the temperature measuring port of the thermal infrared imager is aligned with one of the optical windows for infrared temperature measurement, i.e., the optical windows 112 and 122 and the sample in the reaction chamber are aligned and the surface temperature thereof is measured. The excitation light source is directed at another optical window to illuminate the sample surface.
The atmosphere circulating system comprises a peristaltic pump, a gas chromatograph, a time control switch, a gas cylinder and a flow controller. The peristaltic pump is connected with the gas outlet and the gas chromatograph through a pipeline; the time control switch is connected with the peristaltic pump and is used for controlling the peristaltic pump to be turned on and off at regular time; the flow controller is connected with the gas cylinder and the gas inlet through the gas guide pipe. The flow controller is also connected with the gas chromatograph.
In the above example, the reaction chamber is made of glass, and the sample stage, the thermocouple fixture and the lower cover plate are made of aluminum alloy. The upper cover plate is made of resin materials.
The test atmosphere is formed by mixing the catalyzed organic standard gas and the high-purity dry air through a gas mixing tank and introducing the mixture into a reactor, wherein the ratio of the catalyzed organic standard gas to the high-purity dry air is controlled by a flow controller.
The heating plate can be a German IKA heating plate, and the temperature measurement is an E62.0L infrared thermometer produced by FLIR company and an RS400 temperature display produced in Japan. The light source for photothermal catalysis was a PLS-SXE00 xenon lamp manufactured by Peking Pofel.
The peristaltic pump can be 153Yx/JBT peristaltic pump manufactured by Jencon peristaltic pump company, and the pump pipe is 14 #. The power supply of the power supply is connected with KG316TA for time control.
The reaction gas of the catalytic process can be measured using a gas chromatograph (GC-Smart) manufactured by shimadzu corporation, japan.
The assembly procedure and test method using the reactor of the invention were as follows:
a sample to be measured is manufactured and placed in a sample groove 33 on a sample table, a thermocouple lead is led out from an exhaust port 22 of a reaction cavity, and a clamp 31 on the sample table is matched with a U-shaped lock of M3 type to fix the tip of the thermocouple on the surface of the sample (the tip of a thermocouple wire can be wrapped by the sample to prevent the thermocouple from measuring the temperature of the sample to be received by light and radiation).
The reaction cell is assembled, the optical window sheets 13 and 14 are clamped and sealed by the upper cover plate 11, the lower cover plate 12 and the rubber ring 16, the optical window sheets are fixed by four M6 x 14 hexagonal screws, and the fixed cover plate part is connected with the reaction cavity by four M6 x 30 hexagonal screws.
The assembly of the reaction cell and other accessories is shown in figure 5. The gas source is connected with a tee joint through a flow controller, one port of the tee joint is connected with a gas inlet 21 of the reaction cavity through a pipeline, and the other port of the tee joint is connected with an outlet of the gas chromatograph. The gas outlet 23 of the reaction chamber is connected with the gas inlet of the gas chromatograph by a pipeline through a peristaltic pump, and the power supply of the peristaltic pump is connected with a time control switch. The reaction chamber exhaust port 22 may be connected to the exhaust treatment by a pipe.
The thermocouple lead wire is connected from the exhaust port 22 of the reaction chamber (the exhaust pipeline of the port 22 can be removed in the temperature measurement process) and is fixed by a clamp of the sample table. The assembled reaction cell is placed on a heating plate, a light source is made to face an optical window sheet 13 and shine on a sample, and a camera of an infrared thermometer is aligned with the sample through the optical window sheet 14.
The reactor, the light source, the temperature rising and measuring system and the atmosphere circulating system are assembled according to the scheme. The heating plate is heated to the designated temperature and is kept for half an hour to stabilize the temperature. The cylinder and the vent 22 were opened, the aeration rate was 0.2ml/min for 15min, and the vent 22 was closed.
And controlling the gas chromatograph to start batch analysis, and keeping the peristaltic pump to be always started during the first test so as to remove gas in the reactor and other gases in atmosphere systems such as an air pipe and a GC (gas chromatography). The other test batches regulate and control the time control switch to enable the peristaltic pump to work 0.5min before GC sample injection, close for 1min continuously, keep the closed state for 11min and then open for 1 min. This was recirculated to the end and the reactant and product concentrations were recorded.
The heating plate is heated to the designated temperature and is kept for half an hour to stabilize the temperature. The gas cylinder and the exhaust port 22 are opened, the ventilation rate is 0.2ml/min for 15min, the exhaust port 22 is closed, and the lamp is turned on. The other test procedures were as above.
And after the test is finished, closing the temperature rising and measuring device, the light excitation system, the atmosphere circulating system and the gas chromatograph. And taking down the cover plate, unloading the sample, and cleaning the sample table and the reactor.
Experimental data were recorded and exported for subsequent processing.
Example 2
The photocatalytic reactor and other systems manufactured in example 1 were used, and a gas chromatograph from Shimadzu corporation of Japan was used as an atmosphere detection system, and the sample was P25 powder, the heating plate temperature was 120 ℃, and the gas source was isopropanol and dry air. FIG. 6 is a peak spectrum of isopropanol and catalytically produced acetone detected by a gas chromatograph.
Example 3
Using the photo (thermo) catalytic reactor and other systems fabricated in example 1, the results of detection as shown in FIG. 6 were processed using a gas chromatograph of Shimadzu corporation, Japan, and the peak value and area of each group were individually plotted, FIG. 7(a) is a graph of the results of the test with the addition of a time switch for autonomous injection,
fig. 7(b) is a detection result chart of the time switch not being applied. The data of the time-adding switch has good stability.
FIG. 8 is a graph of the peak area of FIG. 7(a) versus the concentration of converted acetone product in the gaseous standard gas.
Example 4
The photocatalytic reactor prepared in example 1 was used, and a gas chromatograph of Shimadzu corporation, Japan was used as an atmosphere detection system, and the sample was Al2O3For the substrate-supported silver nano-cube, the thermocouple-contacted sample surface at a heating plate temperature of 125 ℃ is shown as 110 ℃ in fig. 10(a), the infrared thermometry calibration emissivity is 0.87, and the dark thermometry is shown as 126 ℃ in fig. 9 (a). 10min after the xenon lamp of PLS-SXE00 was turned on (without a filter, the intensity was adjusted to the minimum), the thermocouple temperature showed 137 ℃ in FIG. 10(b), the infrared temperature measurement showed 144 ℃ in FIG. 9(b), and the temperature of the sample not in the light zone after the lamp was turned on was 127 ℃ in FIG. 9 (c). Because the potassium bromide tablet has the factors of moisture absorption and transmittance reduction, the actual temperature can be obtained by comparing with a group of temperature measuring tables with or without potassium bromide tablets.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (10)
1. A high-controllable high-stability automatic sample introduction type photothermal catalytic reactor is characterized by comprising a cover plate, a reaction chamber and a sample table, wherein the cover plate is covered on the top of the reaction chamber, and the sample table is arranged in the reaction chamber;
the cover plate comprises an upper cover plate and a lower cover plate, two optical windows are arranged on the upper cover plate, and a temperature measuring port of the thermal infrared imager is aligned to one of the optical windows; the excitation light source is aligned with the other optical window;
the side wall of the reaction cavity is provided with an air inlet, an air outlet and an air outlet, wherein the air inlet is connected with an air cylinder, the air outlet is connected with a peristaltic pump, the peristaltic pump is connected with a gas chromatograph through a conduit, and the air inlet is also connected with the gas chromatograph through a pipeline; the exhaust port is used for exhausting residual gas in the reaction cavity and is used as an access port of the thermocouple wire;
and a thermocouple clamp is arranged on the sample table and used for fixing a thermocouple placed from the exhaust port.
2. The highly controllable highly stable autoinjection type photothermal catalytic reactor according to claim 1, wherein the two optical windows are quartz glass and potassium bromide sheets, both of which are sealed and fixed on the cover plate by an O-ring.
3. The highly controllable highly stable autoinjection type photothermal catalytic reactor according to claim 1, wherein the sample stage has a hole in the center and a recess in the bottom for mounting a thermocouple to test the temperature of the backlight area on the bottom of the sample.
4. The highly controllable highly stable autoinjection type photothermal catalytic reactor according to claim 1, wherein the reaction chamber is made of glass material, the sample stage, the thermocouple fixture and the lower cover plate are made of aluminum alloy material, and the upper cover plate is made of resin material.
5. The highly controllable highly stable autoinjection type photothermal catalytic reactor according to claim 1, wherein the upper cover plate and the lower cover plate are tightly fixed on the reaction chamber by screws.
6. The highly controllable highly stable autoinjection type photothermal catalytic reactor according to claim 2, wherein the upper cover plate and the lower cover plate are both provided with grooves for fixing the quartz glass sheet and the potassium bromide sheet.
7. The highly controllable highly stable autoinjection type photothermal catalytic reactor according to claim 1, wherein the exhaust port of the reaction chamber is connected to an exhaust gas treatment device by a pipe.
8. A highly controllable highly stable auto-sampling type photo-thermal catalytic reaction testing device, characterized in that, the testing device comprises the highly controllable highly stable auto-sampling type photo-thermal catalytic reactor of any one of claims 1 to 7, and further comprises an excitation light source, an infrared temperature measurement module and an atmosphere circulating system;
the infrared temperature measuring module comprises a thermocouple, an infrared thermal imager and a heating plate, and the heating plate is arranged below the reaction cavity and used for heating the reaction cavity; the thermocouple is fixed on the surface of the sample through the exhaust port; a temperature measuring port of the thermal infrared imager aligns to one of the optical windows to carry out infrared temperature measurement; the excitation light source is aligned to the other optical window to irradiate the surface of the sample;
the atmosphere circulating system comprises a peristaltic pump, a gas chromatograph, a time control switch, a gas cylinder and a flow controller, wherein the peristaltic pump is connected with a gas outlet and the gas chromatograph through a pipeline; the time control switch is connected with the peristaltic pump and is used for controlling the peristaltic pump to be turned on and off at regular time; the flow controller is connected with the gas cylinder and the gas inlet through the gas guide pipe, reaction gas in the gas cylinder enters the reaction cavity from the gas inlet through the flow controller, the reaction gas is pumped out from the gas outlet through the peristaltic pump and then is guided into the gas chromatograph for detection, and redundant gas is discharged into the reaction cavity from the gas inlet through the pipeline.
9. A highly controllable highly stable auto-sampling type photo-thermal catalytic reaction test method, which is based on the highly controllable highly stable auto-sampling type photo-thermal catalytic reaction test device of claim 8, and comprises the following steps:
(1) preparing a sample to be tested according to the size of the sample table;
(2) placing a sample to be tested into a sample groove in a sample table, placing the sample table into a reaction cavity, fixing the tip of a temperature thermocouple on the surface of the sample through an exhaust port, extending a thermocouple lead out of the reaction cavity, and fixing a cover plate on the reaction cavity;
(3) connecting the gas outlet with a peristaltic pump, pumping out the reaction gas from the gas outlet through the peristaltic pump, introducing the reaction gas into a gas chromatograph for detection, and discharging the redundant gas into the reaction cavity from the gas inlet through a pipeline; discharging residual gas in the reaction chamber from an exhaust port;
(3) adjusting the surface temperature of the sample to a required temperature and stabilizing the surface temperature in a dark state, introducing reaction gas to be detected into the reaction cavity through the gas inlet, and detecting the surface temperature of the sample through one optical window by using a thermal infrared imager after the concentration of the gas in the reaction cavity is stabilized;
(4) starting exciting light, directly irradiating the surface of the sample through another optical window, simultaneously detecting the change of the surface temperature of the sample under the irradiation of the light by using a thermocouple and a thermal infrared imager, and starting a gas chromatograph for automatic cycle test after the surface temperature is stable.
10. The highly controllable highly stable auto-sampling type photothermal catalytic reaction test method according to claim 9, further comprising the steps of:
(5) and after the test is finished, closing the gas chromatograph, the thermocouple and the peristaltic pump, taking out the sample on the sample table, and cleaning the sample table.
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