CN219348775U - Quantitative analysis system for catalytic performance of liquid nitrogen temperature zone normal para-hydrogen catalyst - Google Patents

Quantitative analysis system for catalytic performance of liquid nitrogen temperature zone normal para-hydrogen catalyst Download PDF

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CN219348775U
CN219348775U CN202320518157.8U CN202320518157U CN219348775U CN 219348775 U CN219348775 U CN 219348775U CN 202320518157 U CN202320518157 U CN 202320518157U CN 219348775 U CN219348775 U CN 219348775U
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hydrogen
catalyst
para
fluidized bed
quantitative
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周晗
龚领会
李正宇
柯长磊
杜军军
王倩
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Zhongshan Advanced Cryogenic Technology Research Institute
Technical Institute of Physics and Chemistry of CAS
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Zhongshan Advanced Cryogenic Technology Research Institute
Technical Institute of Physics and Chemistry of CAS
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Abstract

According to the quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst, two groups of fluidized beds are designed, the standard gas catalyst fluidized beds (5) are filled with more catalysts, the flow rate of hydrogen flowing through the fluidized beds is controlled at a lower level, and the para-hydrogen content of outlet hydrogen can be regarded as balanced hydrogen at the temperature of the liquid nitrogen, so that standard gas with known components is obtained; meanwhile, the flow rate of hydrogen flowing through the catalyst quantitative fluidized bed (6) is adjustable, the requirement of quantitative analysis on the catalytic performance of different normal para-hydrogen catalysts under different flow rate conditions is met, the para-hydrogen content analysis unit (140) samples and analyzes sample hydrogen to obtain data related to para-hydrogen content, and further, the catalytic performance of the catalyst can be quantitatively assessed.

Description

Quantitative analysis system for catalytic performance of liquid nitrogen temperature zone normal para-hydrogen catalyst
Technical Field
The utility model relates to the technical field of para-hydrogen gas analysis, in particular to a quantitative analysis system for the catalytic performance of a para-hydrogen catalyst in a liquid nitrogen temperature zone.
Background
The normal hydrogen and the para hydrogen are two spin isomers of molecular hydrogen, and the normal hydrogen spontaneously converts to the para hydrogen at low temperature, but the process is slow, the conversion heat is higher than the vaporization latent heat of liquid hydrogen, and the vaporization of the liquid hydrogen is caused. The normal-para-hydrogen catalyst can accelerate normal-para conversion, and the proportion of para-hydrogen in the liquid hydrogen product can be rapidly increased by using the normal-para-hydrogen catalyst in the hydrogen liquefaction process. The current commercial liquid hydrogen product requires that the ratio of para-hydrogen in the liquid hydrogen is higher than 95%, and a great deal of evaporation of the liquid hydrogen product caused by the conversion heat of natural conversion of the para-hydrogen in the liquid hydrogen storage and transportation process is avoided. To ensure the quality of the liquid hydrogen product, the catalytic performance of the normal para-hydrogen catalyst needs to be quantitatively analyzed and evaluated.
Currently, mainly, a gas chromatograph equipped with a thermal conductivity detector is used as a detection instrument for analysis of para-hydrogen by taking advantage of the difference in thermal conductivity between para-hydrogen and ortho-hydrogen at low temperatures. The needle valve and the float flowmeter on the chromatograph mainframe control the same sample gas quantity sampled each time, and ensure that each analysis is under the same working condition.
The research shows that the sample injection amount of the gas chromatograph has a great influence on analysis results, and the sample injection amount of each analysis needs to be strictly controlled to be the same. The accuracy of the float flowmeter on the chromatograph mainframe is lower, and the operation requirement for experimental staff is higher.
Disclosure of Invention
In view of this, it is necessary to provide a quantitative analysis system for the catalytic performance of a liquid nitrogen Wen Ouzheng para-hydrogen catalyst, which can more conveniently and accurately control the sample injection amount of a chromatograph by an experimenter, aiming at the defects existing in the prior art.
In order to solve the problems, the utility model adopts the following technical scheme:
the utility model provides a quantitative analysis system for the catalytic performance of a positive para-hydrogen catalyst in a liquid nitrogen temperature zone, which comprises the following components: a gas source (110), a gas control unit (120), a vacuum cooling box (130) and a para-hydrogen content analysis unit (140), wherein:
the gas source (110) comprises a hydrogen steel cylinder (1) for storing hydrogen; the hydrogen in the hydrogen steel bottle (1) is supplied to the vacuum cooling box (130) through the gas control unit (120) by a pipeline, and the gas control unit (120) can monitor and control the pressure and flow of the hydrogen flowing through;
the vacuum cooling box comprises a liquid nitrogen dewar (2), a standard gas catalyst fluidized bed (5), a catalyst quantitative fluidized bed (6) and a vacuum dewar (14), wherein a spiral precooling coil (7) is wound on the surface of the standard gas catalyst fluidized bed (5) and the surface of the catalyst quantitative fluidized bed (6), the standard gas catalyst fluidized bed (5), the catalyst quantitative fluidized bed (6) and the spiral precooling coil (7) are arranged in the vacuum dewar (14), the liquid nitrogen dewar (2) provides a cold source for the vacuum dewar (14) through a pipeline, hydrogen in a hydrogen steel bottle (1) is divided into two paths, one path of flow of hydrogen is precooled to the liquid nitrogen temperature through heat exchange between the spiral precooling coil (7) and cold fluid, the standard gas catalyst fluidized bed (5) is cooled through cold hydrogen, the other path of hydrogen is heat exchanged between the spiral precooling coil (7) and the cold fluid to the liquid nitrogen temperature, the standard gas catalyst fluidized bed (6) is precooled through the quantitative pre-cooling coil (6) and the cold fluid to the liquid nitrogen temperature, and the standard gas fluidized bed (6) is connected with the quantitative fluidized bed (140) through the quantitative hydrogen blowing catalyst fluidized bed (6) to the quantitative hydrogen cooling unit for quantitative analysis;
the para-hydrogen content analysis unit (140) analyzes the hydrogen passing through the standard gas catalyst fluidized bed (5) to obtain standard gas with known components, the para-hydrogen content analysis unit (140) analyzes sample gas to be analyzed passing through the catalyst quantitative fluidized bed (6) to obtain para-hydrogen content in the sample hydrogen, and quantitative evaluation is made on the catalytic performance of the catalyst under different flow conditions at liquid nitrogen temperature according to the para-hydrogen content.
In some of these embodiments, the gas control unit (120) includes a pressure reducing valve (11), a needle valve (13), a pressure gauge (3) and a flow meter (4) disposed along the conduit through which the hydrogen gas flows, the pressure gauge (3) and flow meter (4) being configured to monitor the pressure and flow rate of the hydrogen gas, the pressure reducing valve (11) and needle valve (13) being configured to monitor the pressure and flow rate.
In some embodiments, the standard gas catalyst fluidized bed (5) is filled with 4-5ml of catalyst, and the flow rate of hydrogen flowing through the standard gas catalyst fluidized bed (5) is controlled to be 150+/-1 ml/min.
In some of these embodiments, the catalyst metering fluidized bed (6) may be packed with an iron-based normal-para-hydrogen catalyst having a particle size in the range of 200-1000 microns.
In some of these embodiments, the vacuum cold box (130) further comprises a level gauge (8) located within the vacuum dewar (14), the level gauge (8) being used to measure liquid nitrogen position.
In some of these embodiments, the vacuum cooling box (130) further comprises a vacuum pump (9) connected to the vacuum dewar (14), the vacuum pump (9) being used for evacuating the vacuum dewar (14).
In some of these embodiments, the para-hydrogen content analysis unit (140) comprises a gas chromatograph (10), the gas chromatograph (10) being configured to analyze the standard gas data and the sample gas to be analyzed.
By adopting the technical scheme, the utility model has the following beneficial effects:
according to the quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst, two groups of fluidized beds are designed, the standard gas catalyst fluidized beds (5) are filled with more catalysts, the flow rate of hydrogen flowing through the fluidized beds is controlled at a lower level, and the para-hydrogen content of outlet hydrogen can be regarded as balanced hydrogen at the temperature of the liquid nitrogen, so that standard gas with known components is obtained; meanwhile, the flow rate of hydrogen flowing through the catalyst quantitative fluidized bed (6) is adjustable, the requirement of quantitative analysis on the catalytic performance of different normal para-hydrogen catalysts under different flow rate conditions is met, the para-hydrogen content analysis unit (140) samples and analyzes sample hydrogen to obtain data related to para-hydrogen content, and further, the catalytic performance of the catalyst can be quantitatively assessed.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present utility model, the following description will briefly explain the embodiments of the present utility model or the drawings used in the description of the prior art, and it is obvious that the drawings described below are only some embodiments of the present utility model, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst provided in example 1.
Detailed Description
Embodiments of the present utility model are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present utility model and should not be construed as limiting the utility model.
In the description of the present utility model, it should be understood that the directions or positional relationships indicated by the terms "upper", "lower", "horizontal", "inner", "outer", etc., are based on the directions or positional relationships shown in the drawings, are merely for convenience in describing the present utility model and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present utility model.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present utility model, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
The present utility model will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present utility model more apparent.
Example 1
Referring to fig. 1, a flow chart of a quantitative analysis system for the catalytic performance of a positive para-hydrogen catalyst in a liquid nitrogen temperature zone provided by an embodiment of the utility model includes a gas source (110), a gas control unit (120), a vacuum cooling box (130) and a para-hydrogen content analysis unit (140), and the connection and implementation modes of each component are described in detail below.
The gas source (110) comprises a hydrogen steel cylinder (1) for storing hydrogen. High-purity hydrogen is stored in a hydrogen steel cylinder (1).
The hydrogen in the hydrogen steel bottle (1) is supplied to the vacuum cooling box (130) through the gas control unit (120) by a pipeline, and the gas control unit (120) can monitor and control the pressure and flow of the hydrogen flowing through.
In some embodiments, the gas control unit (120) comprises a pressure reducing valve (11), a needle valve (13), a pressure gauge (3) and a flow meter (4) which are arranged on a pipeline through which the hydrogen flows, wherein the pressure gauge (3) and the flow meter (4) are used for monitoring the pressure and the flow rate of the hydrogen, the pressure reducing valve (11) and the needle valve (13) are used for adjusting the pressure and the flow rate, and when the pressure and the flow rate fluctuate greatly, the pressure and the flow rate are adjusted in real time through the pressure reducing valve (11) and the needle valve (13).
The vacuum cooling box comprises a liquid nitrogen Dewar (2), a gas standard catalyst fluidized bed (5), a catalyst quantitative fluidized bed (6) and a vacuum Dewar (14), wherein a spiral pre-cooling coil (7) is wound on the surface of the gas standard catalyst fluidized bed (5) and the surface of the catalyst quantitative fluidized bed (6), and the gas standard catalyst fluidized bed (5), the catalyst quantitative fluidized bed (6) and the spiral pre-cooling coil (7) are arranged in the vacuum Dewar (14). The hydrogen is cooled down by heat exchange between the spiral pre-cooling coil (7) and the hydrogen undergoing the catalytic reaction.
The quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst provided by the embodiment 1 of the utility model has the following working modes:
the liquid nitrogen Dewar (2) provides a cold source for the vacuum Dewar (14) through a pipeline, hydrogen in the hydrogen steel bottle (1) is divided into two paths, one path of flow of hydrogen is pre-cooled to the liquid nitrogen temperature through heat exchange between the spiral pre-cooling coil (7) and cold fluid, the standard gas catalyst fluidized bed (5) is cooled through purging the standard gas catalyst fluidized bed (5) with cold hydrogen, the other path of flow of hydrogen is pre-cooled to the liquid nitrogen temperature through heat exchange between the spiral pre-cooling coil (7) and cold fluid, the catalyst quantitative fluidized bed (6) is cooled through purging the catalyst quantitative fluidized bed (6) with cold hydrogen, and the standard gas catalyst fluidized bed (5) and the catalyst quantitative fluidized bed (6) are respectively connected with the secondary hydrogen content analysis unit (140) through pipelines;
the para-hydrogen content analysis unit (140) analyzes the hydrogen passing through the standard gas catalyst fluidized bed (5) to obtain standard gas with known components, the para-hydrogen content analysis unit (140) analyzes sample gas to be analyzed passing through the catalyst quantitative fluidized bed (6) to obtain para-hydrogen content in the sample hydrogen, and quantitative evaluation is made on the catalytic performance of the catalyst under different flow conditions at liquid nitrogen temperature according to the para-hydrogen content.
It can be understood that the high purity hydrogen cylinders (1) are also directly connected to the para-hydrogen content analysis unit 140, because the analysis of the para-hydrogen analysis instrument (gas chromatograph) requires carrier gas as reference, the present utility model provides 2 high purity hydrogen cylinders (1), one of which provides carrier gas required for the chromatograph analysis; and the other high-purity hydrogen is used as a reaction gas source.
In some embodiments, the standard gas catalyst fluidized bed (5) is filled with 4-5ml of catalyst, and the flow rate of hydrogen flowing through the standard gas catalyst fluidized bed (5) is controlled to be 150+/-1 ml/min. The quantitative fluidized bed (6) of the catalyst can be filled with an iron-based normal-para-hydrogen catalyst with the particle size of 200-1000 microns.
It can be understood that as the analysis principle of the gas chromatograph is that standard gas with known components is needed as a reference to analyze components of sample gas with unknown components, the utility model designs two groups of fluidized beds, namely a standard gas catalyst fluidized bed (5) and a catalyst quantitative fluidized bed (6), the standard gas catalyst fluidized bed (5) is filled with more catalyst, the flow rate of hydrogen flowing through the fluidized bed is controlled at a lower level (150 ml/min, STP), and the secondary hydrogen content of outlet hydrogen can be regarded as balanced hydrogen at the temperature of liquid nitrogen, thus obtaining the standard gas with known components. Meanwhile, the catalyst quantitative fluidized bed (6) with the internal volume of 1ml can be filled with different types of catalysts, the flow of hydrogen flowing through the fluidized bed can be adjusted, and the requirements of quantitative analysis on the catalytic performances of different normal para-hydrogen catalysts under different flow conditions are met. The sample hydrogen is sampled and analyzed on the gas chromatograph 10 to obtain data related to the para-hydrogen content, and further the catalytic performance of the catalyst can be quantitatively assessed.
It can be understood that the standard gas catalyst fluidized bed (5) and the catalyst quantitative fluidized bed (6) are integrated in the same liquid nitrogen vacuum Dewar, so that standard gas and sample gas to be analyzed can be conveniently obtained in the same isothermal environment, and the standard gas and the sample gas are analyzed by a gas chromatograph.
It can be understood that the hydrogen mass flowmeter is adopted to replace the float flowmeter of the chromatograph, so that the measurement of the chromatograph sampling hydrogen flow is performed, and the flow meter of the fluidized bed outlet, the bypass valve and the flow meter of the gas chromatograph outlet are matched with each other, so that the same hydrogen amount during each sample analysis can be controlled more conveniently and accurately.
According to the quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst, two groups of fluidized beds are designed, the standard gas catalyst fluidized beds (5) are filled with more catalysts, the flow rate of hydrogen flowing through the fluidized beds is controlled at a lower level, and the para-hydrogen content of outlet hydrogen can be regarded as balanced hydrogen at the temperature of the liquid nitrogen, so that standard gas with known components is obtained; meanwhile, the flow rate of hydrogen flowing through the catalyst quantitative fluidized bed (6) is adjustable, the requirement of quantitative analysis on the catalytic performance of different normal para-hydrogen catalysts under different flow rate conditions is met, the para-hydrogen content analysis unit (140) samples and analyzes sample hydrogen to obtain data related to para-hydrogen content, and further, the catalytic performance of the catalyst can be quantitatively assessed.
The foregoing description is only of the preferred embodiments of the utility model, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
It will be understood that the technical features of the above-described embodiments may be combined in any manner, and that all possible combinations of the technical features in the above-described embodiments are not described for brevity, however, they should be considered as being within the scope of the description provided in the present specification, as long as there is no contradiction between the combinations of the technical features.
The foregoing description of the preferred embodiments of the present utility model has been provided for the purpose of illustrating the general principles of the present utility model and is not to be construed as limiting the scope of the utility model in any way. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present utility model, and other embodiments of the present utility model as will occur to those skilled in the art without the exercise of inventive faculty, are intended to be included within the scope of the present utility model.

Claims (7)

1. The quantitative analysis system for the catalytic performance of the normal para-hydrogen catalyst in the liquid nitrogen temperature zone is characterized by comprising the following components: a gas source (110), a gas control unit (120), a vacuum cooling box (130) and a para-hydrogen content analysis unit (140), wherein:
the gas source (110) comprises a hydrogen steel cylinder (1) for storing hydrogen; the hydrogen in the hydrogen steel bottle (1) is supplied to the vacuum cooling box (130) through the gas control unit (120) by a pipeline, and the gas control unit (120) can monitor and control the pressure and flow of the hydrogen flowing through;
the vacuum cooling box comprises a liquid nitrogen dewar (2), a standard gas catalyst fluidized bed (5), a catalyst quantitative fluidized bed (6) and a vacuum dewar (14), wherein a spiral precooling coil (7) is wound on the surface of the standard gas catalyst fluidized bed (5) and the surface of the catalyst quantitative fluidized bed (6), the standard gas catalyst fluidized bed (5), the catalyst quantitative fluidized bed (6) and the spiral precooling coil (7) are arranged in the vacuum dewar (14), the liquid nitrogen dewar (2) provides a cold source for the vacuum dewar (14) through a pipeline, hydrogen in a hydrogen steel bottle (1) is divided into two paths, one path of flow of hydrogen is precooled to the liquid nitrogen temperature through heat exchange between the spiral precooling coil (7) and cold fluid, the standard gas catalyst fluidized bed (5) is cooled through cold hydrogen, the other path of hydrogen is heat exchanged between the spiral precooling coil (7) and the cold fluid to the liquid nitrogen temperature, the standard gas catalyst fluidized bed (6) is precooled through the quantitative pre-cooling coil (6) and the cold fluid to the liquid nitrogen temperature, and the standard gas fluidized bed (6) is connected with the quantitative fluidized bed (140) through the quantitative hydrogen blowing catalyst fluidized bed (6) to the quantitative hydrogen cooling unit for quantitative analysis;
the para-hydrogen content analysis unit (140) analyzes the hydrogen passing through the standard gas catalyst fluidized bed (5) to obtain standard gas with known components, the para-hydrogen content analysis unit (140) analyzes sample gas to be analyzed passing through the catalyst quantitative fluidized bed (6) to obtain para-hydrogen content in the sample hydrogen, and quantitative evaluation is made on the catalytic performance of the catalyst under different flow conditions at liquid nitrogen temperature according to the para-hydrogen content.
2. The quantitative analysis system for the catalytic performance of a para-hydrogen catalyst according to claim 1, wherein said gas control unit (120) comprises a pressure reducing valve (11), a needle valve (13), a pressure gauge (3) and a flow meter (4) arranged along a pipe through which said hydrogen gas flows, said pressure gauge (3) and flow meter (4) being used for monitoring the pressure and flow rate of said hydrogen gas, said pressure reducing valve (11) and needle valve (13) being used for regulating said pressure and flow rate.
3. The quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst according to claim 1, wherein the standard gas catalyst fluidized bed (5) is filled with 4-5ml of catalyst, and the flow rate of hydrogen flowing through the standard gas catalyst fluidized bed (5) is controlled to be 150+/-1 ml/min.
4. A quantitative analysis system for the catalytic performance of liquid nitrogen Wen Ouzheng para-hydrogen catalyst according to claim 1, wherein said quantitative fluidized bed (6) of catalyst can be filled with iron-based para-hydrogen catalyst having a particle size ranging from 200 to 1000 microns.
5. The quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst according to claim 1, wherein the vacuum cold box (130) further comprises a liquid level meter (8) positioned in the vacuum dewar (14), and the liquid level meter (8) is used for measuring the position of the liquid nitrogen.
6. The quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst according to claim 1, wherein the vacuum cooling box (130) further comprises a vacuum pump (9) connected with the vacuum dewar (14), and the vacuum pump (9) is used for vacuumizing the vacuum dewar (14).
7. The quantitative analysis system for the catalytic performance of the liquid nitrogen Wen Ouzheng para-hydrogen catalyst according to claim 1, wherein the para-hydrogen content analysis unit (140) comprises a gas chromatograph (10), and the gas chromatograph (10) is used for analyzing standard gas data and sample gas to be analyzed.
CN202320518157.8U 2023-03-09 2023-03-09 Quantitative analysis system for catalytic performance of liquid nitrogen temperature zone normal para-hydrogen catalyst Active CN219348775U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117160369A (en) * 2023-11-01 2023-12-05 中海石油气电集团有限责任公司 Method and device for catalytic conversion of normal-para-hydrogen by continuous and efficient operation of catalyst

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117160369A (en) * 2023-11-01 2023-12-05 中海石油气电集团有限责任公司 Method and device for catalytic conversion of normal-para-hydrogen by continuous and efficient operation of catalyst
CN117160369B (en) * 2023-11-01 2024-04-09 中海石油气电集团有限责任公司 Method and device for catalytic conversion of normal-para-hydrogen by continuous and efficient operation of catalyst

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