Apparatus and method for simultaneous heterogeneous photochemical reactions at different wavelengths

Abstract

The present application relates to the field of heterogeneous photo-reaction, in particular to a device for simultaneously carrying out heterogeneous photochemical reactions under different wavelengths, which comprises a reactor assembly and an optical assembly, the reactor assembly comprises a reaction tube, the reaction tube is a hollow transparent structure, the reaction tube is provided with a reaction gas inlet, a carrier gas inlet and a reaction gas outlet, the reaction gas outlet is connected with an external gas analysis instrument through a pipeline for detecting the composition of the gas after reaction; the optical assembly comprises a light source and a light filtering mechanism, the light filtering mechanism comprises a plurality of sequentially connected light filters, and the wavelengths of the radiation filtered by different light filters are different, the light filtering mechanism is sleeved outside the reaction tube, and the light filtering mechanism can rotate relative to the reaction tube to change the wavelength of the light emitted by the light source into the inside of the reaction tube. The present application can switch different wavelengths in one reaction and detect and analyze the characteristics of heterogeneous photochemical reactions under different wavelengths.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of heterogeneous photo-reaction, in particular to a device and method for simultaneously performing heterogeneous photochemical reactions under different wavelengths. BACKGROUND

[0002] It is reported that the various light-absorbing components contained in atmospheric particulate matter not only have the ability to absorb solar radiation, but also have photochemical reactivity, can be photobleached, or photooxidized into macromolecular compounds; at the same time, atmospheric particulate matter can also uptake SO2, NO2 and other gases in the atmosphere, and undergo more complex heterogeneous photochemical reactions, which are the cause of extreme weather phenomena such as photochemical smog. However, since the sunlight is scattered and refracted multiple times by the atmosphere before it reaches the atmospheric particulate matter, it is difficult to determine the wavelength of the light ultimately absorbed by the particulate matter and involved in the reaction. Further, the composition of atmospheric particulate matter is complex, and different components respond differently to different wavelengths, making it difficult to analyze the photo-reaction of atmospheric particulate matter.

[0003] The heterogeneous photochemical reaction devices on the market can only simulate monochromatic light or one kind of composite light. Since the particulate matter is generally collected on a filter membrane and placed in the reaction device for reaction, only the part facing the light can interact with the light during the reaction. In order to study the effect of different wavelengths on atmospheric particulate matter, it is necessary to emit light of different wavelengths at the same position, but it is not practical to install multiple wavelength lamps at the same position. Frequent replacement of lamps at the same position not only increases the complexity of operation, but also shortens the life of the lamps and their accessories. Therefore, it is difficult to determine the effect of light of different wavelengths on atmospheric particulate matter in the same reaction device. SUMMARY

[0004] In order to compensate for the defects of the existing photochemical reactor, such as being unable to simultaneously perform multi-wavelength reactions and being unable to measure the corresponding reaction light intensity, the present application provides an experimental device capable of simultaneously performing heterogeneous photochemical reactions under different wavelengths, which can switch between different wavelengths in one reaction and detect and analyze the characteristics of heterogeneous photochemical reactions under different wavelengths.

[0005] The present application provides a device for simultaneously performing heterogeneous photochemical reactions under different wavelengths, which comprises a reactor assembly 1, an optical assembly 2 and a sensing assembly 3,

[0006] The reactor assembly 1 comprises a reaction tube 11, which is a hollow transparent structure, and the reaction tube 11 is provided with a reaction gas inlet 12, a carrier gas inlet 13 and a reaction gas outlet 14. The reaction gas outlet is connected to an external gas analysis instrument through a pipeline for detecting the composition of the gas after reaction;

[0007] The optical assembly 2 comprises a light source 21 and a light filter mechanism 22, the light filter mechanism 22 comprises several light filters 23 connected in sequence, and the radiation wavelengths filtered by different light filters are different, the light filter mechanism 22 is sleeved outside the reaction tube 11, and the light filter mechanism 22 can rotate relative to the reaction tube 11 to change the wavelength of the light emitted by the light source 21 into the inside of the reaction tube 11.

[0008] The sensing assembly 3 comprises a detection probe 31, a wire 32 and a display 33 connected in sequence, the detection probe 31 is arranged inside the reaction tube 11, and the wire 32 and the display 33 are arranged outside the reaction tube 11; according to the application, the reactor assembly 1 further comprises a constant temperature tube 15, the constant temperature tube 15 is sleeved outside the reaction tube 11, the constant temperature tube 15 is a hollow structure, and is provided with a constant temperature medium inlet 16 and a constant temperature medium outlet 17, for introducing external constant temperature medium into the inside of the constant temperature tube 15 for circulation, to provide a constant temperature reaction environment for the reaction tube 11, preferably, the constant temperature medium is constant temperature liquid or constant temperature gas, preferably constant temperature liquid, such as water.

[0009] According to the application, the reaction tube 11 and the constant temperature tube 15 are selected from a double-layer quartz flow tube reactor, the constant temperature tube 15 is an outer layer structure, and the reaction tube 11 is an inner layer reaction chamber, and the reaction tube 11 is used for placing a substrate with a sample; preferably, the substrate is a filter membrane, quartz glass and / or calcium fluoride window sheet, and the sample is attached to the substrate by spin coating, deposition or the like.

[0010] According to the application, the reaction gas inlet 12 is provided with a gas guide pipe 18, the gas guide pipe 18 can move in the reaction tube 11 to adjust the position of the reaction gas entering the reaction tube 11; preferably, the gas guide pipe 18 is a movable injection quartz pipe.

[0011] According to the application, the carrier gas inlet 13 is connected with external carrier gas through a pipeline, the carrier gas is mixed with dry gas and wet gas to obtain a gas with a certain humidity, and then the gas is introduced into the carrier gas inlet 13, the wet gas is obtained by introducing the gas into a bubbler filled with deionized water, and the humidity of the carrier gas is adjusted according to the ratio of dry gas / wet gas.

[0012] According to the application, both ends of the reaction tube 11 are provided with sealing members, preferably, the sealing members are composed of sealing rubber rings and sealing heads, and the sealing heads have openings corresponding to the gas guide pipe 18, the reaction gas outlet 14 and the detection probe 31; preferably, the sealing head is a stainless steel sealing head.

[0013] According to the present application, the light source 21 is selected as a composite wavelength lamp tube, the spectrum range of the light source 21 is any wavelength band in 300-800nm; the length of the light source 21 is equivalent to the length of the constant temperature tube 15; preferably, the light source 21 is installed on a lamp holder, and the lamp holder is fixed on a desktop, a wall or other stable position.

[0014] According to the present application, the optical assembly 2 further comprises a bracket 24 and a rotary motor 25 connected with each other, the filter mechanism 22 is arranged on the bracket 24, when the rotary motor 25 drives the bracket 24 to rotate, the filter mechanism 22 rotates with the bracket 24; preferably, the rotary motor 25 is in an infinite adjustable rotation mode or a fixed angle rotation mode; preferably, the filter 23 is a quartz band-pass filter or a filter allowing only light of a certain wavelength to pass through.

[0015] According to the present application, the detection probe 31 is a light intensity detection probe, the detection probe 31 is arranged on the inner bottom of the reaction tube 11, and the end thereof is connected with an external display 33 through a wire 32.

[0016] According to the present application, the reaction gas outlet 14 is connected with a humidity detector and a gas detector through a pipeline, the gas detector comprises SO2 analyzers, NO x analyzers.

[0017] The present application further provides a method for carrying out a heterogeneous photochemical reaction by using the above device, comprising the following steps: attaching a sample on a substrate, putting the sample into the inside of the reaction tube 11, and passing a reaction gas into the reaction tube from the reaction gas inlet 12 to carry out a reaction under a to-be-detected wavelength;

[0018] Preferably, before the reaction, a constant temperature medium is passed into the constant temperature tube 15 to make the temperature in the reaction tube 11 constant;

[0019] Preferably, the filter 23 is adjusted so that the filter 23 of the to-be-detected wavelength corresponds to the light source 21;

[0020] Preferably, the position of the end of the gas guide pipe 18 in the reaction tube 11 is adjusted to adjust the distance between the reaction gas and the particles on the substrate;

[0021] Preferably, during the reaction, the filter 23 can be rotated multiple times to change the wavelength of the light entering the reaction tube 11.

[0022] Advantages

[0023] The device for simultaneously carrying out heterogeneous photochemical reactions under different wavelengths in the application can switch the wavelength of the light reaching the sample surface in the reaction tube by rotating the filter, thereby triggering the photochemical reaction under the wavelength. The temperature in the reaction tube can be strictly controlled by controlling the temperature of the constant temperature medium in the constant temperature tube, and the humidity in the reaction tube can be controlled by adjusting the proportion of dry / humid gas in the carrier, thereby simulating different weather conditions.

[0024] By changing the position of the end of the gas guide pipe at the reaction gas inlet, the relative position of the reaction gas and the sample can be changed, and samples that have undergone photochemical reactions under taken and not taken reaction gases can be obtained at the same time. By detecting the light intensity with a light power sensor, the effects of wavelength and light power on the reaction in the photochemical reaction can be more accurately analyzed, and the research on the heterogeneous photochemical reactions of the sample under different wavelength irradiation at the same time can be realized. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 The figure is a structural schematic diagram of the heterogeneous photochemical reaction device in the application;

[0026] Figure 2 The figure is a top view of the device; Figure 1 The figure is a side view of the device;

[0027] Figure 3 The figure is a side view of the device; Figure 1 The figure is a side view of the device;

[0028] Figure 4 The figure is a structural schematic diagram of a double-layer quartz flow tube;

[0029] Figure 5 The figure is a structural schematic diagram of the filter assembly.

[0030] In the figure: 1-reaction assembly: 11-reaction tube, 12-reaction gas inlet, 13-carrier gas inlet, 14-reaction gas outlet, 15-constant temperature tube, 16-constant temperature medium inlet, 17-constant temperature medium outlet, 18-gas guide pipe;

[0031] 2-optical assembly: 21-light source, 22-filter mechanism, 23-filter, 24-bracket, 25-rotary motor;

[0032] 3-sensing assembly: 31-detection probe, 32-wire, 33-display. DETAILED DESCRIPTION

[0033] The application will be further described in detail below with reference to the accompanying drawings and specific examples. It should be understood that the following examples are only illustrative and explanatory of the application, and should not be interpreted as limiting the scope of protection of the application. Any technology realized based on the above description of the application is covered within the scope of protection intended by the application.

[0034] Example 1

[0035] As Figures 1-5 shown in the schematic diagram of the device that can simultaneously carry out heterogeneous photo-reactions at different wavelengths, including reactor assembly 1, optical assembly 2 and sensing assembly 3, the main part of the reactor assembly 1 is a double-layered quartz flow tube, which is cylindrical, with an inner and outer layer, a length of 500 mm, an inner diameter of 25 mm, the outer layer corresponds to the constant temperature tube 15, and the inner layer corresponds to the reaction tube 11,

[0036] The outer layer of the flow tube is provided with a constant temperature medium inlet 16 and a constant temperature medium outlet 17, the constant temperature medium inlet is connected to the constant temperature medium outlet of the circulating water pump, and the constant temperature medium outlet 17 is connected to the constant temperature medium inlet of the circulating water pump (in this embodiment, the constant temperature medium is water, and in actual operation, other media such as air can also be selected), the water flow is circulated in the outer layer of the flow tube to keep the reaction temperature constant.

[0037] In this embodiment, it is set to 25°C (by keeping the water temperature constant at 25°C), simulating room temperature, and the inside of the flow tube is a reaction chamber where samples collected or spin-coated on glass plates or glass tubes can be placed.

[0038] The left upper end of the double-layered quartz flow tube is provided with a carrier gas inlet 13, the diameter of the carrier gas inlet 13 is set according to the needs, in this embodiment, the diameter is designed to be 6 mm, the carrier gas inlet 13 is connected to the gas cylinder through a polytetrafluoroethylene pipeline, the gas flow is controlled by a mass flow meter, the humidity is fed back in real time by a hygrometer, the flow ratio of dry gas and humid gas through a deionized water bubbler is adjusted to achieve the required humidity for the experiment.

[0039] The left and right sides of the double-layered quartz flow tube are sealed by a sealing rubber ring and a stainless steel sealing head, the inside of the stainless steel sealing head is smoothly polished and can be directly fitted on the double-layered quartz flow tube, the outside of the stainless steel sealing head has threads and can directly tighten the outermost sealing type nut.

[0040] A movable injection quartz tube is installed on the left sealing head to introduce the reaction gas as a reaction gas inlet 12, the inner diameter of the movable injection quartz tube is designed to be 6 mm, and the end part is the reaction gas inlet. Since the injection quartz tube can be manually pushed from the rightmost end to the leftmost end of the reaction chamber, the reaction gas can be introduced into the reaction chamber from any position to complete experiments under different conditions.

[0041] A reaction gas outlet 14 and a wire lead-out port are opened on the right sealing head, the reaction gas outlet 14 connects the gas to a SO2 analyzer, a NOx analyzer and other gas detectors through a polytetrafluoroethylene pipeline, so that the reaction gas can be monitored in real time.

[0042] The optical assembly 2 uses a composite wavelength lamp tube parallel to the quartz flow tube and with similar length, the wavelength range can be 300-800nm or some certain wavelength range, which is similar to the wavelength range of sunlight reaching the ground, which is helpful for analyzing the photochemical reaction occurring in the real atmosphere.

[0043] The lamp tube is installed on the lamp holder, and the lamp tube can be placed above the reactor assembly 1, the filter 23 in the filter mechanism 22 can be a quartz band-pass filter or a filter that only allows light of a certain wavelength to pass, wherein the filter that only allows light of a certain wavelength to pass reflects or absorbs light of other wavelengths when in use, so that only a specific wavelength reaches the sample surface; the rotary motor 25 used in the filter mechanism 22 can be set to an infinitely adjustable rotation mode, or only rotated to a few angles corresponding to the positions of the filters.

[0044] The sensing assembly 3 mainly consists of a light intensity detection probe 31, a wire 32 and a display 33, the light intensity detection probe can be fixed at the lower end of the middle of the reaction chamber, which ensures that the light power of the same position is detected each time, so that the data between experiments are comparable. The wire 32 is led out through the right sealing head, and the sealing ring keeps the seal.

[0045] The assembly method of the above-mentioned heterogeneous photochemical reaction device under different wavelengths is as follows:

[0046] 1. According to the requirements, a double-layer quartz flow tube is made, and a sealing head of corresponding size is custom-made and assembled;

[0047] 2. Custom-made filter 23, metal bracket 24 and rotary motor 25 to form filter mechanism 22;

[0048] 3. Put the light intensity detection probe of the sensing assembly into the double-layer quartz flow tube.

[0049] 4. Put the double-layer quartz flow tube into the filter mechanism 22, fix the lamp tube through the lamp holder above the filter mechanism 22, connect the constant-temperature medium inlet 16 and the constant-temperature medium outlet 17 to the circulating water pump, connect the carrier gas inlet 13 to the carrier gas and mass flowmeter, connect the reaction gas inlet 12 to the reaction gas cylinder and mass flowmeter, and connect the reaction gas outlet 14 to the gas detection instrument.

[0050] The detection method using the above device includes the following steps: attaching the sample to the substrate, placing the substrate inside the reaction tube 11, sealing the reaction tube 11, adjusting the filter 23 so that the filter 23 of the wavelength to be measured corresponds to the light source 21 after the temperature in the reaction tube 11 is constant, and introducing the reaction gas from the reaction gas inlet 12 into the reaction tube for reaction.

[0051] The above describes the embodiments of the present application. However, the present application is not limited to the above-described embodiments. Any modification, equivalent replacement, improvement, and the like made within the spirit and principle of the present application should be included in the scope of protection of the present application.

Claims

1. A device for simultaneously performing heterogeneous photochemical reactions at different wavelengths, characterized in that, The device includes a reactor assembly (1) and an optical assembly (2). The reactor assembly (1) includes a reaction tube (11), which is a hollow and transparent structure. The reaction tube (11) is provided with a reaction gas inlet (12), a carrier gas inlet (13) and a reaction gas outlet (14). The reaction gas outlet (14) is connected to an external gas analyzer through a pipeline to detect the composition of the gas after the reaction. The optical component (2) includes a light source (21) and a filter mechanism (22). The filter mechanism (22) includes several filters (23) connected in sequence, and different filters filter different wavelengths of radiation. The filter mechanism (22) is sleeved on the outside of the reaction tube (11). The filter mechanism (22) can rotate relative to the reaction tube (11) to change the wavelength of the light wave that the light source (21) shines into the reaction tube (11). The device also includes a sensing component (3). The sensing component (3) includes a detection probe (31). The detection probe (31) is set inside the reaction tube (11) and is used to test the light intensity inside the reaction tube (11). The reaction gas inlet (12) is provided with a gas guide tube (18). The gas guide tube (18) can move inside the reaction tube (11) to adjust the position of the reaction gas entering the reaction tube (11). The reaction tube (11) and the thermostatic tube (15) are selected as double-layer quartz flow tube reactors. The thermostatic tube (15) is the outer layer structure, and the reaction tube (11) is the inner reaction chamber. The reaction tube (11) is used to place the substrate with the sample. The substrate is a filter membrane, quartz glass, or calcium fluoride window, and the sample is attached to the substrate by spin coating or deposition.

2. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to claim 1, characterized in that, The sensing component (3) also includes a wire (32) and a display (33). The detection probe (31) is connected to the display (33) via the wire (32). The wire (32) and the display (33) are located outside the reaction tube (11).

3. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to claim 1, characterized in that, The reactor assembly (1) also includes a thermostatic tube (15), which is sleeved on the outside of the reaction tube (11). The thermostatic tube (15) has a hollow structure and is provided with a thermostatic medium inlet (16) and a thermostatic medium outlet (17) for introducing external thermostatic medium into the thermostatic tube (15) for circulation, so as to provide a thermostatic reaction environment for the reaction tube (11).

4. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to claim 3, characterized in that, The constant temperature medium is a liquid or a gas.

5. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to any one of claims 1-4, characterized in that, The air delivery tube (18) is a movable injection quartz tube.

6. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to any one of claims 1-4, characterized in that, The carrier gas inlet (13) is connected to the external carrier gas through a pipeline. The carrier gas is mixed with a dry gas and a wet gas to obtain a gas with a certain humidity before being introduced into the carrier gas inlet (13).

7. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to claim 6, characterized in that, The moisture is obtained by introducing gas into a bubbler containing deionized water, and the humidity of the carrier gas is adjusted according to the dry gas / moist gas ratio.

8. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to any one of claims 1-4, characterized in that, Both ends of the reaction tube (11) are provided with sealing elements, which consist of sealing rings and sealing heads. The sealing heads have openings corresponding to the gas guide tube (18), the reaction gas outlet (14), and the wire (32).

9. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to claim 3, characterized in that, The light source (21) is a composite wavelength lamp tube, and the spectral range of the light source (21) is any band in the range of 300-800 nm.

10. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to claim 9, characterized in that, The length of the light source (21) is equivalent to the length of the thermostatic tube (15); the light source (21) is mounted on a lamp holder, which is fixed to a table or wall.

11. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to any one of claims 1-4, characterized in that, The optical component (2) also includes a bracket (24) and a rotary motor (25) connected to each other. The filter mechanism (22) is mounted on the bracket (24). When the rotary motor (25) drives the bracket (24) to rotate, the filter mechanism (22) rotates with the bracket (24).

12. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to claim 11, characterized in that, The rotary motor (25) is either infinitely adjustable or rotates at a fixed angle each time; the filter (23) is either a quartz bandpass filter or a filter that only allows light of a certain wavelength to pass through.

13. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to any one of claims 1-4, characterized in that, The detection probe (31) is a light intensity detection probe. The detection probe (31) is located at the bottom of the reaction tube (11), and its end is connected to an external display (33) via a wire (32).

14. The apparatus for simultaneously performing heterogeneous photochemical reactions at different wavelengths according to any one of claims 1-4, characterized in that, The reaction gas outlet (14) is connected to a humidity detector and a gas detector via a pipeline. The gas detector includes an SO2 analyzer and a NO analyzer. x Analyzer.

15. A method for performing a heterogeneous photochemical reaction using the apparatus according to any one of claims 1-14, characterized in that, Includes the following steps: The sample is attached to the substrate and placed inside the reaction tube (11). At the wavelength to be measured, the reaction gas is introduced into the reaction tube from the reaction gas inlet (12) to carry out the reaction.

16. The method for heterogeneous photochemical reaction according to claim 15, characterized in that, Before the reaction, a constant temperature liquid / gas is introduced into the constant temperature tube (15) to keep the temperature inside the reaction tube (11) constant; Adjust the filter (23) so that the filter (23) of the wavelength to be measured corresponds to the light source (21); Adjust the position of the end of the gas guide tube (18) inside the reaction tube (11) to adjust the distance between the reaction gas and the particles on the substrate.

17. The method for heterogeneous photochemical reaction according to claim 15, characterized in that, During the reaction, the filter (23) can be rotated multiple times to change the wavelength of the light wave entering the reaction tube (11).

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