CN111189796A - Solid infrared vacuum adsorption characterization system - Google Patents
Solid infrared vacuum adsorption characterization system Download PDFInfo
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- CN111189796A CN111189796A CN202010132302.XA CN202010132302A CN111189796A CN 111189796 A CN111189796 A CN 111189796A CN 202010132302 A CN202010132302 A CN 202010132302A CN 111189796 A CN111189796 A CN 111189796A
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- valve body
- vacuum
- pipeline
- gas
- module
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 36
- 238000012512 characterization method Methods 0.000 title claims abstract description 30
- 239000007787 solid Substances 0.000 title claims abstract description 30
- 238000011065 in-situ storage Methods 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 11
- 230000001502 supplementing effect Effects 0.000 claims abstract description 11
- 238000007664 blowing Methods 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 48
- 239000000523 sample Substances 0.000 description 14
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
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Classifications
-
- 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
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- 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
- G01N21/01—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 a solid infrared vacuum adsorption characterization system, which comprises an air supplementing module, a vacuum module and an in-situ pool module; the air supply module comprises a gas tank and a liquid tank; the vacuum module comprises a vacuum mechanical pump, a molecular turbine pump and a composite vacuum gauge; the in-situ pool module comprises an in-situ pool and a detachable pipeline; the in-situ tank and the vacuum module outlet provided by the invention only need to be connected through one pipeline, so that the in-situ tank and the vacuum module outlet are very convenient; the gas tank and the liquid tank are connected with a gas source, a vacuum mechanical pump and an in-situ pool through valves, and can be vacuumized and inflated; during sample pretreatment, gas source gas directly enters the in-situ cell through the gas supplementing module, the sample is subjected to atmosphere pretreatment at a certain temperature, and then a vacuum pump is started for vacuumizing pretreatment; and then introducing adsorbed gas into the in-situ tank through the gas supplementing module at a certain temperature, and performing infrared characterization after the solid is stably adsorbed, so that the operation is simple and convenient.
Description
Technical Field
The invention relates to the field of catalyst structure characterization instruments, in particular to a solid infrared vacuum adsorption characterization system capable of being used for determining the adsorption state of a solid surface.
Background
The vacuum infrared adsorption is widely used for indirectly characterizing the structure and the property of the catalyst, and can be used for carrying out adsorption characterization on probe molecules on a catalyst sample. For example to realize gases (CO, CO)2NH3, etc.) and liquids (Pyridine, Methanol, Ethanol, H)2O, etc.) and can determine the noble metal structure, valence state, etc. through the characteristic infrared absorption peak of CO adsorptionInformation; the acid-base strength and the amount of acid-base on the sample surface can be determined by the characteristic infrared absorption peak of Pyridine adsorption.
At present, most laboratories adopt a combination device of a vacuum system and an infrared spectrometer, wherein the combination device is made of glass materials researched and developed by large connected objects, but the combination device is very huge and occupies a large area, and the vacuum system is made of glass and is easy to break and disassemble and repair. Compared with the prior art, the metal pool is matched with the vacuum pump set, so that the vacuum pump set has the advantages of convenience in operation, firmness in skin, durability and the like. The applicant applies for the detection device on 20.5.2013, application number 201310187522.2, and the name is a solid surface adsorption infrared detection device made of metal, but an in-situ pool in the device has a complex structure and comprises more than two interfaces, and the device is not easy to install; the mixer is used for filling the adsorption gas, so that the dead volume is large and the cleaning is difficult. And the valve is difficult to realize the switching and continuous use of the whole large pressure range of high vacuum and normal pressure by uniformly using a vacuum valve or a conventional normal pressure valve.
Therefore, how to provide a solid infrared vacuum adsorption characterization system with simple and reasonable structure and convenient operation is a problem that needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
In view of this, the present invention provides a solid infrared vacuum adsorption characterization system, which aims to solve the above technical problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a solid infrared vacuum sorption characterization system, comprising: the system comprises a gas supplementing module, a vacuum module and an in-situ pool module;
the air supply module comprises a gas tank and a liquid tank;
the vacuum module comprises a vacuum mechanical pump, a molecular turbine pump and a composite vacuum gauge;
the in-situ pool module comprises an in-situ pool and a detachable pipeline;
the air exhaust end of the gas tank is connected with an external gas source through a pipeline, and a first valve body is mounted on the air exhaust end; the gas blowing end of the gas tank is connected with the detachable pipeline through a pipeline, and a valve body II, a valve body seventh and a valve body eighth are sequentially arranged on the gas blowing end of the gas tank; the detachable pipeline is communicated with the in-situ tank; the liquid tank is communicated with a pipeline between the second valve body and the seventh valve body through a pipeline, and a third valve body is arranged on the liquid tank; the vacuum mechanical pump is communicated with the molecular turbine pump through a pipeline, and a valve body IV is arranged on the vacuum mechanical pump; the molecular turbopump is communicated with a pipeline between the valve body seven and the valve body eight through a pipeline, is provided with a valve body six, and is communicated with the composite vacuum gauge through a pipeline in an extending way; and the vacuum mechanical pump is communicated with the pipeline between the valve body six and the valve body eight through a pipeline, and a valve body five is arranged on the vacuum mechanical pump.
Through the technical scheme, the in-situ tank and the vacuum module outlet are connected through only one pipeline, and the length of the pipeline can be changed according to the distance between the in-situ tank and the vacuum module and the operation convenience, so that the in-situ tank and the vacuum module outlet are very convenient; the gas tank and the liquid tank are connected with a gas source, a vacuum mechanical pump and an in-situ pool through valves, and can be vacuumized and inflated; during sample pretreatment, gas source gas directly enters the in-situ cell through the gas supplementing module, the sample is subjected to atmosphere pretreatment at a certain temperature, and then a vacuum pump is started for vacuumizing pretreatment; and then introducing adsorbed gas into the in-situ tank through the gas supplementing module at a certain temperature, and performing infrared characterization after the solid is stably adsorbed, so that the operation is simple and convenient.
Preferably, in the above solid infrared vacuum adsorption characterization system, the first valve body, the second valve body and the third valve body are constant pressure valves. Can meet the use requirement.
Preferably, in the above solid infrared vacuum adsorption characterization system, the valve body four, the valve body five, the valve body six, the valve body seven and the valve body eight are vacuum diaphragm valves. The vacuum degree of the pipeline can be improved.
Preferably, in the above solid infrared vacuum adsorption characterization system, the external gas source is a single or multiple steel cylinders or gas bags, and has a detachable interface or a gas distribution box communicated with the first valve body. Can meet the supply requirement of an air source.
Preferably, in the above solid infrared vacuum adsorption characterization system, the external gas source is positive pressure. Can meet the supply requirement of an air source.
Preferably, in the solid infrared vacuum adsorption characterization system, the pipeline in the vacuum module is a vacuum bellows. Can meet the vacuum requirement of the pipeline.
Preferably, in the above solid infrared vacuum adsorption characterization system, the detachable pipe is a corrugated pipe. Can meet the vacuum requirement of the pipeline.
Preferably, in the above solid infrared vacuum adsorption characterization system, the composite vacuum gauge is a pirani vacuum gauge, or consists of a resistance gauge and an ionization gauge. The pressure can be measured.
According to the technical scheme, compared with the prior art, the solid infrared vacuum adsorption characterization system is provided, the in-situ tank and the vacuum module outlet are connected through only one pipeline, the length of the pipeline can be changed according to the distance between the in-situ tank and the vacuum module and the operation convenience, and the system is very convenient; the gas tank and the liquid tank are connected with a gas source, a vacuum mechanical pump and an in-situ pool through valves, and can be vacuumized and inflated; during sample pretreatment, gas source gas directly enters the in-situ cell through the gas supplementing module, the sample is subjected to atmosphere pretreatment at a certain temperature, and then a vacuum pump is started for vacuumizing pretreatment; and then introducing adsorbed gas into the in-situ tank through the gas supplementing module at a certain temperature, and performing infrared characterization after the solid is stably adsorbed, so that the operation is simple and convenient.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic diagram of a system according to the present invention.
Wherein:
1-a gas supplementing module;
11-a gas tank;
12-a liquid tank;
13-valve body one;
14-valve body two;
15-valve body III;
2-a vacuum module;
21-a vacuum mechanical pump;
22-molecular turbopump;
23-a compound vacuum gauge;
24-valve body four;
25-valve body five;
26-valve body six;
27-valve body seven;
28-valve body eight;
3-an in-situ pool module;
31-an in-situ pool;
32-removable pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to the attached figure 1, the embodiment of the invention discloses a solid infrared vacuum adsorption characterization system, which comprises: the system comprises a gas supplementing module 1, a vacuum module 2 and an in-situ tank module 3;
the air supply module 1 comprises a gas tank 11 and a liquid tank 12;
the vacuum module 2 comprises a vacuum mechanical pump 21, a molecular turbine pump 22 and a composite vacuum gauge 23;
the in-situ pool module 3 comprises an in-situ pool 31 and a detachable pipeline 32;
the air exhaust end of the gas tank 11 is connected with an external air source through a pipeline, and a first valve body 13 is installed on the air exhaust end; the gas blowing end of the gas tank 11 is connected with a detachable pipeline 32 through a pipeline, and a valve body II 14, a valve body seventh 27 and a valve body eighth 28 are sequentially arranged on the gas blowing end; the detachable pipeline 32 is communicated with the in-situ tank 31; the liquid tank 12 is communicated with a pipeline between the second valve body 14 and the seventh valve body 27 through a pipeline, and a third valve body 15 is arranged on the liquid tank; the vacuum mechanical pump 21 is communicated with the molecular turbine pump 22 through a pipeline, and a valve body IV 24 is arranged on the vacuum mechanical pump; the molecular turbine pump 22 is communicated with a pipeline between the valve body seven 27 and the valve body eight 28 through a pipeline, a valve body six 26 is arranged on the molecular turbine pump, and the molecular turbine pump is extended and communicated with a composite vacuum gauge 23 through a pipeline; the vacuum mechanical pump 21 is communicated with a pipe between the valve body six 26 and the valve body eight 28 through a pipe, and the valve body five 25 is mounted thereon.
In order to further optimize the technical scheme, the first valve body 13, the second valve body 14 and the third valve body 15 are constant pressure valves.
In order to further optimize the technical scheme, the valve body four 24, the valve body five 25, the valve body six 26, the valve body seven 27 and the valve body eight 28 are vacuum diaphragm valves.
In order to further optimize the technical scheme, the external gas source is a single or a plurality of steel cylinders or gas bags, and is provided with a detachable interface or a gas distribution box which is communicated with the valve body I13.
In order to further optimize the technical scheme, the external air source is positive pressure.
In order to further optimize the above technical solution, the pipe inside the vacuum module 2 is a vacuum bellows.
In order to further optimize the above technical solution, the pipe inside the vacuum module 2 is a vacuum bellows.
In order to further optimize the technical scheme, the composite vacuum gauge 23 is a Pirani vacuum gauge or consists of a resistance gauge and an ionization gauge.
The specific test operation process of the invention is divided into a pretreatment stage and a test stage, wherein the test stage comprises a sample adsorption stage and a sample test stage. The specific process is as follows: closing the valve body III 15, opening the valve body I13, the valve body II 14, the valve body seven 27 and the valve body eight 28, closing other valve bodies, heating the in-situ tank 31 to a certain treatment temperature, introducing gas with a certain pressure into the in-situ tank 31 through an external gas source, closing the valve body II 14 and the valve body seven 27, opening the vacuum mechanical pump 21 and the valve body five 25, vacuumizing the in-situ tank 31 through the vacuum mechanical pump 21, repeatedly inflating and vacuumizing for a plurality of times, so that pretreatment and vacuumizing of a sample in the in-situ tank 31 can be realized, closing the valve body II 14, the valve body seven 27 and the valve body five 25 before the last vacuumizing, and opening the turbo molecular pump 22 and the corresponding valve body four 24 and the valve body six 26 to perform vacuum treatment on the in-situ tank 31. In addition, the in-situ tank 31 can also be directly subjected to vacuum high-temperature pretreatment, after the in-situ tank 31 reaches a certain temperature, the second valve body 14 and the third valve body 15 are closed, the fourth valve body 24, the sixth valve body 26 and the seventh valve body 27 are closed, and the vacuum mechanical pump 21 and the fifth valve body 25 are opened to perform primary vacuum pumping on the in-situ tank 31; after a period of time, valve five 25 is closed and turbomolecular pump 22 and corresponding valve four 24 and valve six 26 are opened to perform a secondary vacuum on in-situ cell 31. After the vacuum pumping is finished, the seventh valve body 27 is opened, the second valve body 14 or the third valve body 15 can be selectively opened, the adsorbed gas or the adsorbed liquid steam with certain pressure can be introduced into the in-situ tank 31, the pressure is measured by the composite vacuum gauge 23, after the sample is adsorbed and balanced, the fourth valve body 24 and the sixth valve body 26 are closed, the fifth valve body 25 is opened to vacuum the in-situ tank 31, so that the adsorbed gas remained in the pipeline of the vacuum module 2 and the in-situ tank 31 and the adsorbed gas with weaker solid surface adsorption can be pumped away, and the infrared absorption characterization can be carried out on the sample. It is to be noted that the background of the sample is measured before the adsorbed gas is introduced into the in situ cell 31, so that after adsorption, the measured signal is reflected as gas adsorption on the surface of the sample.
The device is simple in-situ pool structure, only has one corrugated pipe connector, and the corrugated pipe length can be changed according to the distance between the in-situ pool and the vacuum module and the convenience in operation, and is very convenient. The internal pipeline of the vacuum module is directly adopted to fill the adsorption gas so as to reduce the dead volume, so that the vacuum pump is convenient to extract, or the corrugated pipe is directly removed, and the cleaning is convenient. In addition, the air supply module is connected by a conventional normal pressure valve, the vacuum diaphragm valves are adopted in the vacuum module, the air supply module and the in-situ tank part, the good vacuum degree of the vacuum part is ensured by closing the vacuum diaphragm valves, and the introduction and adsorption of adsorbed gas in the in-situ tank can be realized.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A solid infrared vacuum sorption characterization system, comprising: the system comprises a gas supplementing module (1), a vacuum module (2) and an in-situ tank module (3);
the air supply module (1) comprises a gas tank (11) and a liquid tank (12);
the vacuum module (2) comprises a vacuum mechanical pump (21), a molecular turbopump (22) and a composite vacuum gauge (23);
the in-situ pool module (3) comprises an in-situ pool (31) and a detachable pipeline (32);
the air exhaust end of the gas tank (11) is connected with an external air source through a pipeline, and a first valve body (13) is mounted on the air exhaust end; the gas blowing end of the gas tank (11) is connected with the detachable pipeline (32) through a pipeline, and a valve body II (14), a valve body seventh (27) and a valve body eighth (28) are sequentially arranged on the gas blowing end; the detachable pipeline (32) is communicated with the in-situ tank (31); the liquid tank (12) is communicated with a pipeline between the second valve body (14) and the seventh valve body (27) through a pipeline, and a third valve body (15) is installed on the liquid tank; the vacuum mechanical pump (21) is communicated with the molecular turbine pump (22) through a pipeline, and a valve body IV (24) is mounted on the vacuum mechanical pump; the molecular turbine pump (22) is communicated with a pipeline between the valve body seven (27) and the valve body eight (28) through a pipeline, is provided with a valve body six (26), and is communicated with the composite vacuum gauge (23) through a pipeline in an extending way; the vacuum mechanical pump (21) is communicated with a pipeline between the valve body six (26) and the valve body eight (28) through a pipeline, and a valve body five (25) is installed on the vacuum mechanical pump.
2. The solid infrared vacuum adsorption characterization system of claim 1, wherein the first valve body (13), the second valve body (14), and the third valve body (15) are constant pressure valves.
3. The solid infrared vacuum adsorption characterization system of claim 1, wherein the valve body four (24), the valve body five (25), the valve body six (26), the valve body seven (27), and the valve body eight (28) are vacuum diaphragm valves.
4. The solid state infrared vacuum adsorption characterization system of claim 1, wherein the external gas source is one or more steel cylinders or gas bags, and has a detachable interface or gas distribution box in communication with the first valve body (13).
5. The solid infrared vacuum adsorption characterization system of claim 1, wherein the external gas source is positive pressure.
6. A solid infrared vacuum adsorption characterization system according to claim 1, wherein the conduit within the vacuum module (2) is a vacuum bellows.
7. A solid infrared vacuum adsorption characterization system according to claim 1, wherein the detachable tube (32) is a bellows.
8. The solid infrared vacuum adsorption characterization system of claim 1, wherein the composite vacuum gauge (23) is a pirani vacuum gauge or is composed of a resistance gauge and an ionization gauge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010132302.XA CN111189796A (en) | 2020-02-29 | 2020-02-29 | Solid infrared vacuum adsorption characterization system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010132302.XA CN111189796A (en) | 2020-02-29 | 2020-02-29 | Solid infrared vacuum adsorption characterization system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111189796A true CN111189796A (en) | 2020-05-22 |
Family
ID=70706788
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010132302.XA Pending CN111189796A (en) | 2020-02-29 | 2020-02-29 | Solid infrared vacuum adsorption characterization system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111189796A (en) |
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2020
- 2020-02-29 CN CN202010132302.XA patent/CN111189796A/en active Pending
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