CN114624206A - In-situ infrared device based on modulation excitation spectrum - Google Patents
In-situ infrared device based on modulation excitation spectrum Download PDFInfo
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- CN114624206A CN114624206A CN202011464197.6A CN202011464197A CN114624206A CN 114624206 A CN114624206 A CN 114624206A CN 202011464197 A CN202011464197 A CN 202011464197A CN 114624206 A CN114624206 A CN 114624206A
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- infrared
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- pool
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 54
- 238000000695 excitation spectrum Methods 0.000 title claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 69
- 239000000243 solution Substances 0.000 claims abstract description 31
- 239000013078 crystal Substances 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000011949 solid catalyst Substances 0.000 claims abstract description 13
- 230000001276 controlling effect Effects 0.000 claims abstract description 11
- 230000001105 regulatory effect Effects 0.000 claims abstract description 5
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 description 7
- 238000002329 infrared spectrum Methods 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 4
- 210000005056 cell body Anatomy 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
Abstract
The invention discloses an in-situ infrared device based on a modulation excitation spectrum, belongs to the technical field of instruments and equipment, and can solve the problems of complex structure and high use cost of the conventional in-situ infrared device. The device comprises: the liquid mixing unit is used for mixing the first solution and the second solution and regulating and controlling the mixing ratio of the first solution and the second solution so as to ensure that the concentration of the mixed solution is changed periodically; the in-situ infrared pool comprises a cylindrical pool body with an opening at the bottom end, an infrared crystal for closing the opening at the bottom end of the cylindrical pool body, and a solid catalyst which is positioned in the cylindrical pool body and fixed on the infrared crystal; the infrared light beam can be totally reflected in the infrared crystal; a liquid inlet and a liquid outlet are arranged on the side wall of the cylindrical tank body; the mixed solution flows into the cylindrical tank body from the liquid inlet, reacts with the solid catalyst in situ and flows out from the liquid outlet. The invention is used for modulating the excitation spectrum.
Description
Technical Field
The invention relates to an in-situ infrared device based on a modulation excitation spectrum, and belongs to the technical field of instruments and equipment.
Background
Modulation of excitation spectroscopy is a class of surface characterization techniques that have been developed in recent years and can be paired with a variety of in situ characterization techniques. The excitation spectrum is modulated mainly by regulating and controlling periodic changes of parameters related to the reaction, such as pressure, concentration, Ph and the like, and observing changes of signals obtained by an in-situ characterization technology so as to analyze the mechanism of the catalytic reaction. The technique can be matched with various in-situ characterization techniques, such as a total reflection in-situ infrared technique.
The total reflection infrared (ATR-IR) technique developed in recent years is an effective in-situ characterization technique for detecting a solid-liquid interface, and can detect an infrared absorption spectrum by internal reflection of a crystal, and when an incident angle is larger than a critical angle, total reflection occurs, and a part of light penetrates through a part of the surface of the crystal to a depth and is absorbed by a sample between specific frequencies, so that an infrared spectrum is finally formed. The combination of ATR-IR with modulated excitation spectra allows accurate identification of intermediate species of catalytic reactions and the like. However, most of the existing in-situ infrared devices are complex in structure and high in use cost.
Disclosure of Invention
The invention provides an in-situ infrared device based on a modulation excitation spectrum, which can solve the problems of complex structure and higher use cost of the conventional in-situ infrared device.
The invention provides an in-situ infrared device based on modulation excitation spectrum, which comprises: the liquid mixing unit is used for mixing a first solution with a second solution and regulating and controlling the mixing ratio of the first solution to the second solution so as to enable the concentration of the mixed solution to be changed periodically; the in-situ infrared pool comprises a cylindrical pool body with an opening at the bottom end, an infrared crystal for closing the opening at the bottom end of the cylindrical pool body, and a solid catalyst which is positioned in the cylindrical pool body and fixed on the infrared crystal; the infrared light beam can be totally reflected in the infrared crystal; a liquid inlet and a liquid outlet are formed in the side wall of the cylindrical tank body; and the mixed solution flows into the cylindrical tank body from the liquid inlet, reacts with the solid catalyst in situ and flows out from the liquid outlet.
Optionally, the apparatus further comprises a liquid pump disposed between the liquid mixing unit and the in-situ infrared pool; the liquid pump is used for conveying the mixed solution mixed by the liquid mixing unit into the in-situ infrared pool.
Optionally, the liquid mixing unit includes a first container, a first output pipeline connected to the first container, a second output pipeline connected to the second container, and a mixing pipeline communicated with output ends of the first output pipeline and the second output pipeline; the output end of the mixing pipeline is communicated with the input end of the liquid pump; the first container contains a first solution; a second solution is contained in the second container; the first output pipeline is provided with a first valve, and the first valve is used for controlling the output flow rate of the first solution; and a second valve is arranged on the second output pipeline and used for controlling the output flow rate of the second solution.
Optionally, the apparatus further comprises an overflow unit, an inlet of the overflow unit is connected with an output end of the liquid pump; the outlet of the overflow unit is connected with the liquid inlet of the in-situ infrared pool; the outlet of the overflow unit is flat, and the outlet of the overflow unit is matched with the shape of the liquid inlet of the in-situ infrared pool.
Optionally, the outlet width of the overflow unit is equal to the width of the infrared crystal.
Optionally, the overflow unit includes a receiving box and an overflow pipe; the first end of the overflow pipe is inserted into the accommodating box from the bottom end of the accommodating box, and the second end of the overflow pipe is connected with the liquid inlet of the in-situ infrared pool; the side wall of the containing box is provided with a liquid inlet, and the liquid inlet is connected with the output end of the liquid pump.
Optionally, the infrared crystal is any one of zinc selenide, silicon, diamond and germanium.
Optionally, the working temperature of the in-situ infrared pool is-20 ℃ to 500 ℃.
Optionally, the concentration variation waveform of the mixed solution is any one of a sine wave, a cosine wave, a square wave and a triangular wave.
Optionally, the first valve and/or the second valve is a solenoid valve.
The invention can produce the beneficial effects that:
(1) the invention provides an in-situ infrared device based on modulation excitation spectrum, which mainly comprises a liquid mixing unit and an in-situ infrared pool. A liquid mixing unit in the device mainly controls two strands of solutions to be mixed through an electromagnetic valve control system, a material flow with a certain concentration change is formed within a certain time, so that a periodic signal is formed, and a rule that a solid catalyst surface signal changes along with the concentration in an in-situ infrared pool is detected through an infrared spectrum detection device to obtain a modulation excitation spectrum. The device can realize the modulation excitation spectrum on the total reflection infrared device, and has simple structure and lower use cost.
(2) According to the in-situ infrared device based on the modulation excitation spectrum, the overflow unit is arranged between the liquid pump and the in-situ infrared pool, and the outlet of the overflow unit is flat and has the same width as the infrared crystal, so that the liquid with different concentrations can be ensured to uniformly flow through the surface of the solid catalyst.
Drawings
FIG. 1 is a schematic structural diagram of an in-situ infrared device based on modulated excitation spectrum according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an overflow unit according to an embodiment of the present invention;
FIG. 3 is an IR spectrum of cyclohexanol measured in accordance with an embodiment of the present invention;
FIG. 4 is a modulated excitation spectrum with square wave modulation for the spectral signal at 2980cm-1 provided by an embodiment of the present invention.
List of parts and reference numerals:
11. a first container; 12. a second container; 13. a first valve; 14. a second valve; 15. a liquid pump; 16. an overflow unit; 161. a containing box; 162. an overflow pipe; 17. a cylindrical tank body; 18. an infrared crystal; 19. a solid catalyst; 20. an infrared beam; 21. and (5) sealing rings.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited to these examples.
An embodiment of the present invention provides an in-situ infrared device based on a modulated excitation spectrum, as shown in fig. 1, the device includes: the liquid mixing unit is used for mixing the first solution and the second solution and regulating and controlling the mixing ratio of the first solution and the second solution so as to ensure that the concentration of the mixed solution is changed periodically; the in-situ infrared pool comprises a cylindrical pool body 17 with an opening at the bottom end, an infrared crystal 18 for closing the opening at the bottom end of the cylindrical pool body 17, and a solid catalyst 19 which is positioned in the cylindrical pool body 17 and fixed on the infrared crystal 18; the infrared beam 20 may be totally reflected within the infrared crystal 18; a liquid inlet and a liquid outlet are arranged on the side wall of the cylindrical tank body 17; the mixed solution flows into the cylindrical tank body 17 from the liquid inlet, reacts with the solid catalyst 19 in situ and flows out from the liquid outlet.
The concentration variation waveform of the mixed solution may be any one of a sine wave, a cosine wave, a square wave, and a triangular wave, which is not limited in the embodiment of the present invention.
In practical application, the in-situ infrared cell can be used together with infrared equipment such as an infrared spectrum detector and the like. FIG. 3 is an infra-red spectrum of cyclohexanol measured; FIG. 4 is for 2980cm-1The spectrum signal is subjected to square wave modulation excitation spectrum, wherein the period T of the square wave is 240 s.
In an embodiment of the present invention, the infrared crystal 18 may be any one of zinc selenide, silicon, diamond, and germanium.
In practical application, the working temperature of the in-situ infrared pool is generally-20 ℃ to 500 ℃.
Further, the device also comprises a liquid pump 15 arranged between the liquid mixing unit and the in-situ infrared pool; the liquid pump 15 is used for conveying the mixed solution mixed by the liquid mixing unit into the in-situ infrared pool.
Referring to fig. 1, the liquid mixing unit includes a first container 11, a first output pipeline connected to the first container 11, a second container 12, a second output pipeline connected to the second container 12, and a mixing pipeline communicated with output ends of the first output pipeline and the second output pipeline; the output end of the mixing pipeline is communicated with the input end of the liquid pump 15; the first container 11 contains a first solution; a second container 12 contains a second solution; the first output pipeline is provided with a first valve 13, and the first valve 13 is used for controlling the output flow rate of the first solution; the second output pipeline is provided with a second valve 14, and the second valve 14 is used for controlling the output flow rate of the second solution. Wherein the first valve 13 and/or the second valve 14 may be solenoid valves.
In the invention, the in-situ infrared device mainly comprises a liquid mixing unit, a liquid pump 15 and an in-situ infrared pool. A liquid mixing unit in the device mainly controls two strands of solutions to be mixed through an electromagnetic valve control system, a material flow with a certain concentration change is formed within a certain time, so that a periodic signal is formed, and a rule that a surface signal of a solid catalyst 19 in an in-situ infrared pool changes along with the concentration is detected through an infrared spectrum detection device, so that a modulation excitation spectrum is obtained. The device can realize the modulation excitation spectrum on the total reflection infrared device, has simple structure and lower use cost.
Further, referring to fig. 1 and 2, the device further comprises an overflow unit 16, wherein an inlet of the overflow unit 16 is connected with an output end of the liquid pump 15; the outlet of the overflow unit 16 is connected with the liquid inlet of the in-situ infrared pool; the outlet of the overflow unit 16 is flat, and the outlet of the overflow unit 16 is matched with the liquid inlet of the in-situ infrared pool in shape. Wherein, the overflow unit 16 may include a receiving box 161 and an overflow pipe 162; a first end of the overflow pipe 162 is inserted into the accommodating box 161 from the bottom end of the accommodating box 161, and a second end of the overflow pipe 162 is connected with a liquid inlet of the in-situ infrared pool; the side wall of the accommodating box 161 is provided with a liquid inlet, and the liquid inlet is connected with the output end of the liquid pump 15. The outlet width L of the overflow unit 16 is equal to the width of the infrared crystal 18.
According to the invention, the overflow unit 16 is arranged between the liquid pump 15 and the in-situ infrared pool, and as the outlet of the overflow unit 16 is flat and has the same width as the infrared crystal 18, the liquid with different concentrations can be ensured to uniformly flow through the surface of the solid catalyst 19.
In the embodiment of the invention, the in-situ infrared cell further comprises a sealing ring 21, and the sealing ring 21 is used for sealing the joint of the cylindrical cell body 17 and the infrared crystal 18, so that the reaction solution in the cylindrical cell body 17 can be prevented from leaking from the joint of the simple cell body 17 and the infrared crystal 18. The seal ring 21 may be an O-ring rubber seal ring 21.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. An in-situ infrared device based on modulated excitation spectra, the device comprising:
the liquid mixing unit is used for mixing a first solution with a second solution and regulating and controlling the mixing ratio of the first solution to the second solution so as to ensure that the concentration of the mixed solution is periodically changed;
the in-situ infrared pool comprises a cylindrical pool body with an opening at the bottom end, an infrared crystal for closing the opening at the bottom end of the cylindrical pool body, and a solid catalyst which is positioned in the cylindrical pool body and fixed on the infrared crystal; the infrared light beam can be totally reflected in the infrared crystal; a liquid inlet and a liquid outlet are formed in the side wall of the cylindrical tank body; and the mixed solution flows into the cylindrical tank body from the liquid inlet, reacts with the solid catalyst in situ and flows out from the liquid outlet.
2. The apparatus of claim 1, further comprising a liquid pump disposed between the liquid mixing unit and the in-situ infrared cell;
the liquid pump is used for conveying the mixed solution mixed by the liquid mixing unit into the in-situ infrared pool.
3. The apparatus of claim 2, wherein the mixing unit comprises a first container, a first output conduit connected to the first container, a second output conduit connected to the second container, and a mixing conduit in communication with output ends of the first output conduit and the second output conduit; the output end of the mixing pipeline is communicated with the input end of the liquid pump;
the first container contains a first solution; a second solution is contained in the second container;
the first output pipeline is provided with a first valve, and the first valve is used for controlling the output flow rate of the first solution;
and a second valve is arranged on the second output pipeline and used for controlling the output flow rate of the second solution.
4. The apparatus of claim 2, further comprising an overflow unit, an inlet of the overflow unit being connected to an output of the liquid pump; the outlet of the overflow unit is connected with the liquid inlet of the in-situ infrared pool;
the outlet of the overflow unit is flat, and the outlet of the overflow unit is matched with the shape of the liquid inlet of the in-situ infrared pool.
5. The apparatus of claim 4, wherein the overflow unit has an outlet width equal to a width of the infrared crystal.
6. The apparatus of claim 4 or 5, wherein the overflow unit comprises a containment box and an overflow pipe; the first end of the overflow pipe is inserted into the accommodating box from the bottom end of the accommodating box, and the second end of the overflow pipe is connected with the liquid inlet of the in-situ infrared pool;
the side wall of the containing box is provided with a liquid inlet, and the liquid inlet is connected with the output end of the liquid pump.
7. The apparatus of claim 1, wherein the infrared crystal is any one of zinc selenide, silicon, diamond, and germanium.
8. The apparatus of claim 1, wherein the in-situ infrared cell has an operating temperature of-20 ℃ to 500 ℃.
9. The apparatus according to claim 1, wherein the concentration variation waveform of the mixed solution is any one of a sine wave, a cosine wave, a square wave, and a triangular wave.
10. The device of claim 3, wherein the first valve and/or the second valve is a solenoid valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011464197.6A CN114624206A (en) | 2020-12-10 | 2020-12-10 | In-situ infrared device based on modulation excitation spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011464197.6A CN114624206A (en) | 2020-12-10 | 2020-12-10 | In-situ infrared device based on modulation excitation spectrum |
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| Publication Number | Publication Date |
|---|---|
| CN114624206A true CN114624206A (en) | 2022-06-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011464197.6A Pending CN114624206A (en) | 2020-12-10 | 2020-12-10 | In-situ infrared device based on modulation excitation spectrum |
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| Country | Link |
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| CN (1) | CN114624206A (en) |
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2020
- 2020-12-10 CN CN202011464197.6A patent/CN114624206A/en active Pending
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