Device for preparing standard gases with different deuterium abundance

Abstract

The present application provides a device for preparing standard gases of different deuterium abundance, comprising: a feeding unit for providing natural water, the natural water comprising deuterium water and hydrogen water; the electrolytic hydrogen production unit is used for electrolyzing natural water to generate standard gas, and the standard gas comprises hydrogen and deuterium gas; the water-hydrogen liquid-phase catalytic exchange unit comprises a first feed port, a catalytic exchange column and a second feed port which are sequentially communicated in the first direction, the first feed port is used for transmitting standard gas to the catalytic exchange column, and the second feed port is used for transmitting natural water to the catalytic exchange column; the deuterium gas and the hydrogen water in the catalytic exchange column are subjected to a hydrogen isotope exchange reaction, and standard gas with deuterium abundance decreasing in sequence in the first direction is obtained; the catalytic exchange column comprises at least two discharge ports which are sequentially formed in the first direction, and the deuterium abundance of standard gas output by any two discharge ports is different. According to the device disclosed by the invention, standard gases with different deuterium abundance can be obtained at the same time through a method of combining liquid-phase catalytic exchange with electrolysis.

Description

Technical Field

[0001] This application relates to the field of preparation technology, and in particular to an apparatus for preparing standard gases with different deuterium abundances. Background Technology

[0002] This section is intended to provide background or context for the implementation of this application. The description herein should not be construed as an admission that it is prior art.

[0003] Standard gases of varying deuterium abundances provide researchers with a stable reference for accurately calibrating equipment, validating experimental methods, exploring isotope effects, and tracking the dynamics of water molecules in fields such as chemical analysis, environmental monitoring, biological research, and nuclear technology. This ensures the reliability of experimental results and the precision of scientific research. The application needs of standard gases of varying deuterium abundances are mainly concentrated in the following areas: 1) Calibrating the sensitivity and resolution of mass spectrometers. By using standard gases with known deuterium abundances, the ion source, ion optics system, and detector of mass spectrometers can be calibrated to ensure the accuracy of measurement results; 2) The distribution of deuterium in the atmosphere can serve as an indicator of environmental changes, reflecting the source and migration path of water vapor. This allows standard gases of varying deuterium abundances to be used to develop and calibrate environmental monitoring technologies, helping scientists better understand environmental changes; 3) In nuclear fusion experiments, [the following applies to] non-deuterium [other applications]. Standard gases with the same deuterium abundance can be used to simulate the deuterium fuel environment in nuclear fusion reactions, helping to optimize reaction conditions and improve fusion efficiency; 4) In the process of optical fiber manufacturing, deuterium gas can be used to prevent hydrogen-induced loss in optical fibers, and standard gases with different deuterium abundances can be used to study the diffusion and fixation mechanisms of deuterium in optical fibers to optimize the manufacturing process of optical fibers; 5) In the biomedical field, deuterium gas can be used to synthesize deuterated drugs to improve drug stability and bioavailability, and standard gases with different deuterium abundances can also be used to calibrate analytical instruments in the pharmaceutical process to ensure the quality control of deuterated drugs.

[0004] Therefore, standard gases with different deuterium abundances have a wide range of applications in analytical instrument calibration, nuclear physics research, geochemistry, environmental science and industrial applications. The use of these standard gases helps to improve the accuracy of measurements, optimize experimental conditions and promote the development of related fields.

[0005] In related technologies, the water-hydrogen dual-temperature exchange method is commonly used to prepare deuterium gas. This method uses two reactors at different temperatures: a high-temperature reactor and a low-temperature reactor. In the high-temperature reactor, hydrogen gas reacts with deuterium-water, and hydrogen atoms in the hydrogen gas exchange with deuterium atoms in the deuterium-water to generate a standard gas containing deuterium. In the low-temperature reactor, the exchange reaction between deuterium-water and hydrogen gas proceeds in reverse, promoting the separation of deuterium gas. To obtain standard gases with different deuterium abundances, multiple preparations need to be performed by adjusting the reaction parameters. Therefore, developing a preparation technology that can simultaneously obtain standard gases with different deuterium abundances is of great significance. Summary of the Invention

[0006] In view of this, the main objective of this application is to provide an apparatus for preparing standard gases with different deuterium abundances. The apparatus of this application, through a liquid-phase catalytic exchange combined with electrolysis method, can simultaneously obtain standard gases with different deuterium abundances, and the deuterium abundance can be precisely controlled, thereby enabling the rapid preparation of standard gases with different deuterium abundances according to the required deuterium abundance.

[0007] To achieve the above objectives, this application provides the following technical solution.

[0008] This application provides an apparatus for preparing standard gases with different deuterium abundances, comprising: The feeding unit is used to provide natural water, including deuterium water and hydrogen water; The electrolysis hydrogen production unit is used to electrolyze natural water to generate standard gases, which include hydrogen and deuterium. A water-hydrogen liquid-phase catalytic exchange unit includes a first feed inlet, a catalytic exchange column, and a second feed inlet connected sequentially in a first direction. The end of the first feed inlet furthest from the catalytic exchange column is connected to an electrolytic hydrogen production unit, used to transfer standard gas provided by the electrolytic hydrogen production unit to the catalytic exchange column. The end of the second feed inlet furthest from the catalytic exchange column is connected to a feed unit, used to transfer natural water provided by the feed unit to the catalytic exchange column. The catalytic exchange column is used to catalyze the hydrogen isotope exchange reaction between deuterium and hydrogen water to obtain a standard gas with decreasing deuterium abundance along a first direction. The catalytic exchange column includes at least two outlets arranged sequentially along the first direction, and the deuterium abundance of the standard gas output from any two outlets is different.

[0009] In some embodiments, the catalytic exchange column includes: a shell having a receiving cavity; a packing material disposed within the receiving cavity, the packing material comprising at least two layers of packing material stacked along a first direction, a catalyst layer disposed between adjacent packing layers and / or between the packing layer and the shell, the catalyst layer comprising a hydrophobic catalyst, and the packing layer comprising a hydrophilic packing material; the ratio of the total volume of the catalyst layer to the total volume of the packing layer is (1:1)-(1:4).

[0010] In some embodiments, the hydrophobic catalyst includes a support and an active component. The support includes at least one of styrene-divinylbenzene copolymer, polytetrafluoroethylene, molecular sieve, and ceramic, and / or the active component includes platinum metal; and / or the hydrophilic filler includes at least one of triangular spiral filler, Dixon filler, Canon filler, and calendered ring filler.

[0011] In some embodiments, the average particle size of the hydrophobic catalyst is 1 mm to 5 mm.

[0012] In some embodiments, the average particle size of the hydrophilic filler is 1 mm to 5 mm.

[0013] In some embodiments, at least one filler layer satisfies the following condition: the ratio of the thickness of the filler layer in the first direction to the average particle size of the hydrophilic filler contained in the filler layer is 1-3.

[0014] In some embodiments, at least one catalyst layer satisfies the following condition: the ratio of the thickness of the catalyst layer in the first direction to the average particle size of the hydrophobic catalyst contained in the catalyst layer is 1-3.

[0015] In some embodiments, the ratio of the average particle size of the hydrophilic filler contained in the filling layer to the average particle size of the hydrophobic catalyst contained in the adjacent catalyst layer is (1:1)-(2:1).

[0016] In some embodiments, the apparatus for preparing standard gases with different deuterium abundances further includes at least two cooling units, each connected to an outlet, the cooling units being used to remove water vapor from the standard gases output from the outlets.

[0017] In some embodiments, the apparatus for preparing standard gases with different deuterium abundances further includes at least two drying units, each of which is connected to a cooling unit, and the drying units are used to dry the standard gases cooled by the cooling units.

[0018] In some embodiments, the apparatus for preparing standard gases with different deuterium abundances further includes at least two product units, each product unit being connected to a drying unit. The product units are used to store the standard gases output from the drying unit and to detect the deuterium abundance of the standard gases.

[0019] In some embodiments, the apparatus for preparing standard gases with different deuterium abundances further includes a circulating heat-insulating water unit disposed on the circumferential surface of the water-hydrogen liquid-phase catalytic exchange unit, the circulating heat-insulating water unit being used to regulate the temperature of the water-hydrogen liquid-phase catalytic exchange unit.

[0020] The apparatus for preparing standard gases with different deuterium abundances according to this application includes a feed unit, an electrolytic hydrogen production unit, and a water-hydrogen liquid-phase catalytic exchange unit. The standard gas produced by the electrolytic hydrogen production unit is transferred to the catalytic exchange column in the water-hydrogen liquid-phase catalytic exchange unit through a first feed port, while natural water provided by the feed unit is transferred to the catalytic exchange column through a second feed port. Deuterium in the standard gas and hydrogen water in the natural water undergo a hydrogen isotope exchange reaction in the catalytic exchange column, transferring deuterium from the deuterium gas to the hydrogen water, thereby obtaining standard gases with deuterium abundance decreasing sequentially along a first direction. The catalytic exchange column includes at least two outlets arranged sequentially along the first direction, thereby allowing the acquisition of standard gases with different deuterium abundances from each outlet.

[0021] The apparatus of this application for preparing standard gases with different deuterium abundances can simultaneously obtain standard gases with different deuterium abundances through a liquid-phase catalytic exchange combined with electrolysis method, and the deuterium abundance can be precisely controlled, thereby enabling the rapid preparation of standard gases with different deuterium abundances according to the requirements of hydrogen deuterium abundance.

[0022] In addition to the technical problems solved by this disclosure, the technical features constituting the technical solutions, and the beneficial effects brought about by the technical features of these technical solutions as described above, other technical problems that this disclosure can solve, other technical features contained in the technical solutions, and the beneficial effects brought about by these technical features will be further described in detail in the following specific embodiments. Attached Figure Description

[0023] To more clearly illustrate the technical solutions in the embodiments of this application or the conventional technology, the drawings used in the description of the embodiments or the conventional technology will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0024] Figure 1 A schematic diagram of an apparatus for preparing standard gases with different deuterium abundances according to an embodiment of this application is shown.

[0025] Explanation of reference numerals in the attached figures 1. Feeding unit; 11. Natural water; 2. Water-hydrogen liquid-phase catalytic exchange unit; 21. First feed inlet; 22. Catalytic exchange column; 221. Outlet; 221a. Outlet; 221b. Outlet; 221c. Outlet; 221y. Outlet; 221z. Outlet; 23. Second feed inlet; 3. Electrolysis hydrogen production unit; 31. Standard gas; 4. Cooling unit; 5. Drying unit; 6. Product unit. Detailed Implementation

[0026] The technical solution of this disclosure will be clearly and completely described below with reference to specific embodiments and accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this disclosure, and not all of them. Based on the embodiments in this disclosure, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0027] Throughout this specification, unless otherwise specified, the terminology used herein shall be understood as having the meaning as commonly used in the art. Therefore, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In the event of any conflict, this specification shall prevail.

[0028] It should be noted that, in this disclosure, the term "comprising" or any other variation thereof is intended to cover non-exclusive inclusion, such that a method or apparatus that comprises a list of elements includes not only the elements expressly stated, but also other elements not expressly listed, or elements inherent to implementing the method or apparatus. Without further limitations, an element defined by the phrase "containing..." does not exclude the presence of other related elements in the method or apparatus that includes that element.

[0029] The above steps are only for clarity. In practice, they can be combined into one step or some steps can be broken down into multiple steps. As long as they include the same logical relationship, they are all within the scope of protection of this patent.

[0030] Terminology Definition As used in this article, the term “deuterium” is an isotope of hydrogen, also known as heavy hydrogen.

[0031] As used in this article, the term "deuterium abundance" refers to the ratio of the number of deuterium atoms to the number of ordinary hydrogen atoms in a given sample or system. Deuterium abundance is usually expressed as the number of deuterium atoms per million hydrogen atoms (D / H ratio). Since the content of deuterium is generally low, deuterium abundance is usually expressed in ppm (parts per million).

[0032] In related technologies, the water-hydrogen dual-temperature exchange method is commonly used to prepare standard gases. To prepare a standard gas with a specified deuterium abundance, precise control of reaction parameters is required, such as reaction temperature and material circulation flow rate. Among these, reaction temperature significantly affects the rate and equilibrium position of the hydrogen isotope exchange reaction; higher temperatures favor the reaction towards the formation of the standard gas, while lower temperatures facilitate the separation of the standard gas. The material circulation flow rate affects the residence time of the reactants in the system, thus influencing the completeness of the hydrogen isotope exchange reaction. Lower flow rates result in longer reactant residence times, more complete hydrogen isotope exchange, and higher deuterium abundance in the standard gas.

[0033] To meet the demand for preparing standard gases with different deuterium abundances, parameters such as reaction temperature and material circulation flow rate need to be controlled. Controlling these parameters is complex, and since only a specific reaction condition can be adjusted each time to obtain a standard gas with one deuterium abundance, preparing a series of standard gases with different deuterium abundances requires multiple adjustments of reaction parameters and multiple preparations, increasing operational complexity and time costs. Therefore, developing a technology capable of simultaneously obtaining standard gases with different deuterium abundances is of great significance.

[0034] Based on this, this application provides an apparatus for preparing standard gases with different deuterium abundances. Please refer to [link to relevant documentation]. Figure 1 The device includes: a feeding unit 1, a water-hydrogen liquid-phase catalytic exchange unit 2, and an electrolysis hydrogen production unit 3.

[0035] Feeding unit 1 is used to provide natural water 11, which includes deuterated water and hydrogen water; electrolysis hydrogen production unit 3 is used to electrolyze natural water 11 to generate standard gas 31, which includes hydrogen and deuterium; water-hydrogen liquid phase catalytic exchange unit 2 includes a first feed port 21, a catalytic exchange column 22 and a second feed port 23 connected in sequence in a first direction. The end of the first feed port 21 away from the catalytic exchange column 22 is connected to the electrolysis hydrogen production unit 3 and is used to transfer the standard gas 31 provided by the electrolysis hydrogen production unit 3 to the catalytic exchange column 22. The end of the second feed port 23 away from the catalytic exchange column 22 is connected to the feeding unit 1 and is used to transfer the natural water 11 provided by the feeding unit 1 to the catalytic exchange column 22. The catalytic exchange column 22 is used to catalyze the hydrogen isotope exchange reaction between hydrogen water in natural water 11 and deuterium gas in standard gas 31 to obtain standard gas with deuterium abundance decreasing sequentially along the first direction. The catalytic exchange column includes at least two outlets 221 arranged sequentially along the first direction, and the deuterium abundance of the standard gas output from any two outlets 221 is different.

[0036] This application does not specifically limit the source of the natural water 11. For example, it can be municipal water, river water, or seawater. The natural water includes hydrogen water (H2O) and deuterium water (HDO and D2O). The deuterium content in the natural water is approximately 0.015‰ (i.e., 15 mg / kg or 15 ppm).

[0037] In this application, standard gas refers to a mixture of hydrogen and deuterium.

[0038] In this application, the term "deuterium abundance" refers to the ratio of the number of deuterium atoms to the number of ordinary hydrogen atoms in a standard gas.

[0039] The following describes the working process of the apparatus for preparing standard gases with different deuterium abundances provided in the embodiments of this application.

[0040] Feed unit 1 provides natural water 11, which enters through the second inlet 23 of the water-hydrogen liquid-phase catalytic exchange unit 2 and is transported to the catalytic exchange column 22. In the catalytic exchange column 22, a hydrogen isotope exchange reaction occurs to generate deuterium-rich water. The generated deuterium-rich water flows from the catalytic exchange column 22 into the electrolytic hydrogen production unit 3, where it is electrolyzed to generate standard gas 31 and oxygen. Standard gas 31 enters through the first inlet 21 of the water-hydrogen liquid-phase catalytic exchange unit 2 and is transported to the catalytic exchange column 22. In the catalytic exchange column 22, standard gas 31 and natural water 11 undergo a hydrogen isotope exchange reaction, transferring deuterium from the standard gas 31 to the natural water 11. Since the standard gas 31 enters from the first feed port 21, as the standard gas 31 is transported along the first direction, the degree of hydrogen isotope exchange reaction between the natural water 11 and the standard gas 31 gradually increases. Therefore, standard gas with deuterium abundance decreasing sequentially along the first direction is obtained, so that standard gas with different deuterium abundance can be output from each discharge port 221.

[0041] The apparatus for preparing standard gases with different deuterium abundances disclosed in this application utilizes a liquid-phase catalytic exchange combined with electrolysis method to simultaneously obtain standard gases with different deuterium abundances. Furthermore, the deuterium abundance can be precisely controlled, thereby enabling the rapid preparation of standard gases with different deuterium abundances according to the required deuterium abundance of the standard gas.

[0042] According to some embodiments, the catalytic exchange column 22 includes at least two outlets 221 arranged sequentially along a first direction. For example, when N outlets 221 are provided, N standard gases with different deuterium abundances can be obtained from each outlet 221.

[0043] See also Figure 1 The outlet 221 closest to the first feed inlet 21 is outlet 221a, and the outlet 221 closest to the second feed inlet 23 is outlet 221z.

[0044] The deuterium abundance of the standard gas output from outlet 221z is less than that of the standard gas output from outlet 221y, which is less than... less than that of the standard gas output from outlet 221c, which is less than that of the standard gas output from outlet 221b, which is less than that of the standard gas output from outlet 221a. In other words, the deuterium abundance of the standard gas output from outlet 221z is the lowest, and the deuterium abundance of the standard gas output from outlet 221a is the highest.

[0045] It should be noted that the number N of discharge ports 221 can be adaptively adjusted according to the required deuterium abundance range of the standard gas, where N is an integer greater than or equal to 2. For example, N can be 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, etc.

[0046] According to some embodiments, a catalytic exchange column includes: a shell having a receiving cavity; and a packing material disposed within the receiving cavity, comprising at least two layers of packing material stacked along a first direction, wherein a catalyst layer is disposed between adjacent packing layers and / or between the packing layer and the shell, the catalyst layer comprising a hydrophobic catalyst, and the packing layer comprising a hydrophilic packing material. The hydrophobic catalyst can accelerate the exchange reaction between hydrogen isotopes, promoting the occurrence of the catalytic exchange reaction. The introduction of the hydrophilic packing material increases the contact area between hydrogen water and deuterium gas, thereby further promoting the exchange reaction between hydrogen isotopes, thereby generating standard gases with different deuterium abundances.

[0047] Depending on the gas (standard gas 31) throughput, the hydrophobic catalyst can be either particulate or ordered. When the standard gas 31 throughput is small, the corresponding natural water flow rate is also small, in which case a particulate catalyst can be selected; when the standard gas 31 throughput is large, the corresponding natural water flow rate is also large, in which case an ordered catalyst is required to reduce pressure drop.

[0048] In this application, "regular structure catalyst" refers to a catalyst with a defined geometric shape, such as a cube or octahedron, which is usually uniformly and orderly arranged.

[0049] In this application, "particulate catalyst" is usually a randomly arranged fine particle, which is a catalyst with irregular shape and different size.

[0050] The type of hydrophilic packing is selected based on the processing capacity of standard gas 31. For example, when the processing capacity of standard gas 31 is small, bulk packing is generally selected, including but not limited to stainless steel mesh ring packing; when the processing capacity of standard gas 31 is large, structured packing is generally selected, usually stainless steel structured packing, including but not limited to stainless steel corrugated packing, etc.

[0051] In this application, "bulk filler" typically refers to small, irregularly shaped particles. These fillers vary in shape and size and are usually manufactured through processes such as pressing and sintering.

[0052] In this application, "structured packing" refers to packing with regular geometric shapes, such as metal corrugated plate packing and plastic corrugated plate packing. Their ordered structure is typically achieved through specific design to improve mass transfer efficiency.

[0053] According to some embodiments, the hydrophobic catalyst includes a support and an active component. The support is used to load the active component, under the action of the active component, hydrogen water in natural water 11 and deuterium gas in standard gas 31 undergo a hydrogen isotope exchange reaction.

[0054] According to some embodiments, the support includes at least one of styrene-divinylbenzene copolymer (SDB), polytetrafluoroethylene (PTFE), molecular sieve, and ceramic, and the active component includes the noble metal platinum. Exemplarily, the hydrophobic catalyst includes at least one of Pt-SDB (supported by polystyrene-divinylbenzene copolymer and supported by platinum) and Pt-PTFE (supported by polytetrafluoroethylene and supported by platinum metal).

[0055] According to some embodiments, the hydrophilic packing includes at least one of triangular spiral packing, Dixon packing, Canon packing, and calendered ring packing.

[0056] According to some embodiments, the ratio of the total volume of the catalyst layer to the total volume of the packing layer is (1:1) to (1:4). By adjusting the ratio of the total volume of the catalyst layer to the total volume of the packing layer, the contact area between the active surface of the hydrophobic catalyst and natural water can be controlled, thereby affecting the rate and extent of deuterium exchange. A volume ratio of the catalyst layer to the packing layer within the above range is beneficial for precisely controlling the deuterium abundance of the prepared standard gas. Exemplarily, the volume ratio of the hydrophobic catalyst to the hydrophilic packing is 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, or any value within a range of two such values, but is not limited thereto.

[0057] According to some embodiments, the average particle size of the hydrophobic catalyst is 1 mm to 5 mm. This is beneficial for increasing the contact area between the catalyst layer and the standard gas, while reducing the flow resistance of the catalyst layer to natural water, thereby achieving higher exchange efficiency while ensuring a high hydrogen isotope exchange reaction rate. Exemplarily, the average particle size of the hydrophobic catalyst is a value between 1 mm, 2 mm, 3 mm, 4 mm, 5 mm, or any two of these values.

[0058] According to some embodiments, the average particle size of the hydrophilic filler is 1mm-5mm, which helps to increase the contact area between the filler layer and natural water, while reducing the flow resistance of the filler layer to the standard gas. This ensures both a high hydrogen isotope exchange reaction rate and higher exchange efficiency. For example, the average particle size of the hydrophilic filler is 1mm, 2mm, 3mm, 4mm, 5mm, or a value within a range of any two of these values.

[0059] According to some embodiments, at least one packing layer satisfies the following condition: the ratio of the thickness of the packing layer in the first direction to the average particle size of the hydrophilic packing material contained in the packing layer is 1-3. This allows for the placement of more packing layers within a limited container space. This increase in layered structure facilitates better contact between the natural water and the standard gas, resulting in more hydrogen isotope exchanges. This also allows for precise control of the deuterium abundance in the final standard gas while improving exchange efficiency. For example, the ratio of the thickness of the packing layer in the first direction to the average particle size of the hydrophilic packing material contained in the packing layer is a value between 1, 1.5, 2, 2.5, 3, or any two of these values.

[0060] According to some embodiments, at least one catalyst layer satisfies the following condition: the ratio of the thickness of the catalyst layer in the first direction to the average particle size of the hydrophobic catalyst contained in the catalyst layer is 1-3. This allows for the placement of more catalyst layers within a limited container space. This increased layered structure facilitates better contact between the natural water and the standard gas, resulting in more hydrogen isotope exchanges. This also allows for precise control of the deuterium abundance in the final standard gas while improving exchange efficiency. For example, the ratio of the thickness of the catalyst layer in the first direction to the average particle size of the hydrophobic catalyst contained in the catalyst layer is a value between 1, 1.5, 2, 2.5, 3, or any two of these values.

[0061] According to some embodiments, the ratio of the average particle size of the hydrophilic filler in the packing layer to the average particle size of the hydrophobic catalyst in the adjacent catalyst layer is (1:1) to (2:1). This facilitates the flow and distribution of natural water and standard gas between the packing layer and the catalyst layer, allowing natural water and standard gas to pass through each layer more uniformly, thereby increasing the exchange rate of hydrogen isotopes. For example, the ratio of the average particle size of the hydrophilic filler in the packing layer to the average particle size of the hydrophobic catalyst in the adjacent catalyst layer is 1:1, 1.2:1, 1.4:1, 1.5:1, 1.6:1, 1.8:1, 2:1, or any value within a range of two such ratios.

[0062] It should be noted that, based on the required deuterium abundance range of the standard gas, the thickness of the catalyst layer, the number of catalyst layers, the type of hydrophobic catalyst, the average particle size of the hydrophobic catalyst, the thickness of the packing layer, the number of packing layers, the type of hydrophilic packing, the average particle size of the hydrophilic packing, and the diameter of the catalytic exchange column can be adaptively adjusted, thereby achieving precise control of deuterium abundance and enabling the rapid preparation of standard gases with different deuterium abundances that meet the requirements.

[0063] According to some implementation methods, please refer to Figure 1 The apparatus for preparing standard gases with different deuterium abundances further includes at least two cooling units 4, each cooling unit 4 being connected to an outlet 221. The cooling units 4 are used to remove water vapor from the standard gases output from the outlet 221. The cooling units 4 can cool the standard gases output from the outlet 221 of the water-hydrogen liquid-phase catalytic exchange unit 2, removing saturated water vapor. This application does not specifically limit the cooling method; exemplarily, cooling can be performed using circulating cooling water.

[0064] According to some implementation methods, please refer to Figure 1The apparatus for preparing standard gases with different deuterium abundances further includes at least two drying units 5, each drying unit 5 being connected to a cooling unit 4. The drying units 5 are used to dry the standard gases cooled by the cooling units 4. The drying units 5 mainly perform deep drying on the cooled standard gases to remove moisture and avoid the influence of moisture on the deuterium abundance. This application embodiment does not specifically limit the drying method; exemplarily, drying can be performed using silica gel columns.

[0065] According to some implementation methods, please refer to Figure 1 The apparatus for preparing standard gases with different deuterium abundances also includes at least two product units 6, each product unit 6 connected to a drying unit 5. The product units 6 store the standard gases output from the drying unit 5 and detect the deuterium abundance of the standard gases. The product units 6 first receive standard gases with different deuterium abundances output from the drying unit 5, and then analyze and compare the received standard gases. The accurate deuterium abundance in the standard gases is obtained through mass spectrometry analysis; this deuterium abundance value is the deuterium abundance of each standard gas. The product units 6 then store each standard gas with determined deuterium abundance separately. This storage can be achieved by compressing the standard gases into gas cylinders using hydrogen storage, or by storing them in alloy materials using metal hydrogen storage. When needed, the standard gases can be released directly from the corresponding hydrogen storage cylinder or alloy.

[0066] According to some embodiments, the apparatus for preparing standard gases with different deuterium abundances further includes a circulating heat-insulating water unit (not shown) disposed on the circumferential surface of the water-hydrogen liquid-phase catalytic exchange unit 2. The circulating heat-insulating water unit is used to regulate the temperature of the water-hydrogen liquid-phase catalytic exchange unit 2. The water-hydrogen liquid-phase catalytic exchange unit 2 needs to maintain a certain temperature to ensure high efficiency and uniformity of hydrogen isotope exchange. Therefore, by setting up a circulating heat-insulating water unit to heat the water-hydrogen liquid-phase catalytic exchange unit 2, the temperature inside the water-hydrogen liquid-phase catalytic exchange unit 2 is maintained at a suitable reaction temperature.

[0067] According to some implementation methods, when the diameter of the catalytic exchange column 22 is small, an electric heating method can also be used to provide a suitable reaction temperature for the water-hydrogen liquid phase catalytic exchange unit 2.

[0068] Example The following describes embodiments of this application. The embodiments described below are exemplary and are only used to explain this application, and should not be construed as limiting this application. Where specific techniques or conditions are not specified in the embodiments, they are performed according to the techniques or conditions described in the literature in this field or according to the product instructions. Reagents or instruments used, unless otherwise specified, are all conventional products that can be obtained commercially.

[0069] Example 1 The standard gas produced by the electrolysis hydrogen production unit enters the catalytic exchange column through the first inlet, while the natural water from the feed unit enters the catalytic exchange column through the second inlet. The catalytic exchange column is a stainless steel reaction column, filled with a mixture of hydrophobic catalyst and hydrophilic packing material. The hydrophobic catalyst is a granular platinum-based hydrophobic catalyst (average particle size 1.8 mm), with each catalyst layer 2 mm thick in the first direction. The hydrophilic packing material is bulk stainless steel Dixon packing (average particle size 2 mm), with each packing layer 6 mm thick in the first direction. There are 17 packing layers and 17 catalyst layers. The total volume of the hydrophobic catalyst and hydrophilic packing material is 9 L. Deuterium from the standard gas and hydrogen from the natural water undergo a hydrogen isotope exchange reaction within the catalytic exchange column, transferring deuterium from the deuterium gas to the hydrogen water. The catalytic exchange column has five outlets along a first direction. The outlet closest to the first inlet is the first outlet, and the outlet closest to the second inlet is the fifth outlet. The outlets are arranged sequentially along the first direction: first outlet, second outlet, third outlet, fourth outlet, and fifth outlet. The standard gas output from the fifth outlet has a deuterium abundance of 60 ppm, the fourth outlet has 200 ppm, the third outlet has 400 ppm, the second outlet has 800 ppm, and the first outlet has 1000 ppm. The standard gas output from each outlet is cooled to room temperature (25°C) by a cooling unit, then passes through a drying unit and enters the product unit, where it is stored using an alloy hydrogen storage system.

[0070] Example 1 can prepare standard gases with deuterium abundance ranging from 60 ppm to 1000 ppm.

[0071] Example 2 The standard gas produced by the electrolysis hydrogen production unit enters the catalytic exchange column through the first inlet, while the natural water from the feed unit enters the catalytic exchange column through the second inlet. The catalytic exchange column is a stainless steel reaction column, filled with a mixture of hydrophobic catalyst and hydrophilic packing material. The hydrophobic catalyst is a structured platinum-based hydrophobic catalyst (average particle size 5 mm), with each catalyst layer having a thickness of 10 mm in the first direction. The hydrophilic packing material is a structured stainless steel corrugated packing material, with each packing layer having a thickness of 40 mm in the first direction. There are 30 packing layers and 30 catalyst layers, with a total volume of 900 L for both the hydrophobic catalyst and hydrophilic packing material. Deuterium from the standard gas and hydrogen from the natural water undergo a hydrogen isotope exchange reaction within the catalytic exchange column, transferring deuterium from the deuterium gas to the hydrogen water. The catalytic exchange column has ten outlets arranged along a first direction. The outlet closest to the first inlet is the first outlet, the outlet closest to the second inlet is the tenth outlet, and the outlets are arranged sequentially along the first direction as follows: first outlet, second outlet, third outlet, fourth outlet, fifth outlet, sixth outlet, seventh outlet, eighth outlet, ninth outlet, and tenth outlet. Example 2 can prepare standard gases with deuterium abundances ranging from 100 ppm to 2000 ppm.

[0072] As can be seen from the two specific embodiments above, the apparatus for preparing standard gases with different deuterium abundances in this application obtains the standard gases through a combined electrolysis method of liquid-phase catalytic exchange of deuterium and hydrogen water. Furthermore, the catalytic exchange column of this apparatus includes at least two outlets arranged sequentially along a first direction. By precisely controlling the thickness of the catalyst layer, the number of catalyst layers, the type of hydrophobic catalyst, the average particle size of the hydrophobic catalyst, the thickness of the packing layer, the number of packing layers, the type of hydrophilic packing, and the average particle size of the hydrophilic packing, the deuterium abundance of the standard gases can be precisely controlled. Thus, standard gases with different deuterium abundances can be obtained simultaneously from each outlet, rapidly preparing standard gases with different deuterium abundances to meet specific requirements.

[0073] The above descriptions are merely some specific embodiments of this disclosure, intended to illustrate this disclosure, and are not intended to limit the scope of protection claimed in this application. Any modifications or substitutions made based on the inventive concept of this disclosure and the content of this application's specification and drawings, or direct / indirect applications in other related technical fields, are included within the scope of protection claimed in this application.

Claims

1. An apparatus for preparing standard gases with different deuterium abundances, characterized in that, include: A feeding unit for providing natural water, including deuterium water and hydrogen water; An electrolysis hydrogen production unit is used to electrolyze the natural water to generate standard gas, the standard gas including hydrogen and deuterium; A water-hydrogen liquid-phase catalytic exchange unit includes a first feed inlet, a catalytic exchange column, and a second feed inlet connected sequentially in a first direction. The end of the first feed inlet furthest from the catalytic exchange column is connected to an electrolytic hydrogen production unit, used to transfer the standard gas provided by the electrolytic hydrogen production unit to the catalytic exchange column. The end of the second feed inlet furthest from the catalytic exchange column is connected to a feed unit, used to transfer the natural water provided by the feed unit to the catalytic exchange column. The catalytic exchange column is used to catalyze the hydrogen isotope exchange reaction between the deuterium gas and the hydrogen water to obtain the standard gas with the deuterium abundance decreasing sequentially along the first direction. The catalytic exchange column includes at least two outlets arranged sequentially along the first direction, and the deuterium abundance of the standard gas output from any two outlets is different.

2. The apparatus according to claim 1, characterized in that, The catalytic exchange column comprises: The outer casing has a receiving cavity; A filler is disposed within the receiving cavity. The filler comprises at least two filler layers stacked along the first direction. A catalyst layer is disposed between two adjacent filler layers and / or between the filler layer and the outer shell. The catalyst layer comprises a hydrophobic catalyst. The filler layer comprises a hydrophilic filler. The ratio of the total volume of the catalyst layer to the total volume of the filler layer is (1:1) to (1:4).

3. The apparatus according to claim 2, characterized in that, The hydrophobic catalyst comprises a support and an active component, wherein the support comprises at least one selected from styrene-divinylbenzene copolymer, polytetrafluoroethylene, molecular sieve, and ceramic, and / or the active component comprises platinum; and / or, The hydrophilic packing includes at least one of triangular spiral packing, Dixon packing, Canon packing, and calendered ring packing.

4. The apparatus according to claim 3, characterized in that, The average particle size of the hydrophobic catalyst is 1 mm to 5 mm, and / or the average particle size of the hydrophilic filler is 1 mm to 5 mm.

5. The apparatus according to claim 4, characterized in that, At least one of the filler layers satisfies the following condition: the ratio of the thickness of the filler layer in the first direction to the average particle size of the hydrophilic filler contained in the filler layer is 1-3, and / or, At least one of the catalyst layers satisfies the following condition: the ratio of the thickness of the catalyst layer in the first direction to the average particle size of the hydrophobic catalyst contained in the catalyst layer is 1-3.

6. The apparatus according to claim 4, characterized in that, The ratio of the average particle size of the hydrophilic filler contained in the filling layer to the average particle size of the hydrophobic catalyst contained in the adjacent catalyst layer is (1:1)-(2:1).

7. The apparatus according to any one of claims 1 to 6, characterized in that, It also includes at least two cooling units, each of which is connected to one of the discharge ports. The cooling unit is used to remove water vapor from the standard gas output from the outlet.

8. The apparatus according to claim 7, characterized in that, It also includes at least two drying units, each of which is connected to one of the cooling units. The drying unit is used to dry the standard gas after it has been cooled by the cooling unit.

9. The apparatus according to claim 8, characterized in that, It also includes at least two product units, each of which is connected to one of the drying units. The product unit is used to store the standard gas output from the drying unit and to detect the deuterium abundance of the standard gas.

10. The apparatus according to claim 9, characterized in that, It also includes a circulating heat-insulating water unit disposed on the circumferential surface of the water-hydrogen liquid-phase catalytic exchange unit. The circulating heat-insulating water unit is used to regulate the temperature of the water-hydrogen liquid-phase catalytic exchange unit.

Images