CN115716661A - Method for producing oxygen 16-enriched metal oxide - Google Patents
Method for producing oxygen 16-enriched metal oxide Download PDFInfo
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- 238000000034 method Methods 0.000 claims abstract description 54
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- 238000002360 preparation method Methods 0.000 claims abstract description 18
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- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
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- QVGXLLKOCUKJST-IGMARMGPSA-N oxygen-16 atom Chemical compound [16O] QVGXLLKOCUKJST-IGMARMGPSA-N 0.000 abstract 7
- QVGXLLKOCUKJST-NJFSPNSNSA-N oxygen-18 atom Chemical compound [18O] QVGXLLKOCUKJST-NJFSPNSNSA-N 0.000 description 44
- UTDLAEPMVCFGRJ-UHFFFAOYSA-N plutonium dihydrate Chemical compound O.O.[Pu] UTDLAEPMVCFGRJ-UHFFFAOYSA-N 0.000 description 43
- FLDALJIYKQCYHH-UHFFFAOYSA-N plutonium(IV) oxide Inorganic materials [O-2].[O-2].[Pu+4] FLDALJIYKQCYHH-UHFFFAOYSA-N 0.000 description 43
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 34
- HRBJILZCKYHUJF-UHFFFAOYSA-J [Pu+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O Chemical compound [Pu+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O HRBJILZCKYHUJF-UHFFFAOYSA-J 0.000 description 30
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- 238000006243 chemical reaction Methods 0.000 description 20
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
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- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 description 9
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- QVGXLLKOCUKJST-OUBTZVSYSA-N oxygen-17 atom Chemical compound [17O] QVGXLLKOCUKJST-OUBTZVSYSA-N 0.000 description 7
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- QNJPYBOCFFOTGM-UHFFFAOYSA-J [Cl-].[Cl-].[Cl-].[Cl-].[Pu+4] Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Pu+4] QNJPYBOCFFOTGM-UHFFFAOYSA-J 0.000 description 6
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- 150000000703 Cerium Chemical class 0.000 description 1
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Images
Abstract
The application provides a preparation method of a metal oxide enriched with oxygen 16, which can be applied to the technical field of isotope heat source process preparation. The method for producing the oxygen 16-enriched metal oxide comprises the following steps: preparing a salt solution of the metal using the oxygen 16 enriched water; adding an oxygen 16-enriched oxalic acid solution to the salt solution to obtain an oxygen 16-enriched oxalate precipitate of the metal; calcining the oxalate precipitate in oxygen 16 enriched oxygen to produce the oxygen 16 enriched metal oxide.
Description
Technical Field
The application relates to the technical field of isotope heat source process preparation, in particular to a preparation method of metal oxide enriched with oxygen 16.
Background
Plutonium 238 belongs to the group of alpha decay synthases, and high-energy alpha particles are released during the decay process of plutonium 238, and these particles react with surrounding substances to generate heat energy. By using this characteristic, a certain amount of 238 PuO 2 The core block is prepared by the process, and then the core block is welded and sealed by a high-temperature resistant alloy cladding and encapsulated by a carbon-carbon composite material, so that an isotope heat source (RHU) can be obtained. The method is characterized in that an RHU is used as an energy source, a thermoelectric converter is arranged around the RHU, a plutonium 238 isotope battery is obtained through battery shell packaging, and the plutonium 238 isotope battery is mainly used for deep space exploration. Due to the fact that 238 PuO 2 The oxygen element in the natural environment comes from the air in the nature, so the oxygen element in the natural environment comes from the air in the nature 238 PuO 2 The medium oxygen mainly consists of oxygen 16, oxygen 17 and oxygen 18. And the oxygen 17 and the oxygen 18 have the probability of generating neutrons and radiation by reaction, so that 238 PuO 2 Has high neutron emissivity, which has great influence on the life of the deep space probe and the life health of astronauts, and has more oxygen 18 than 17, so that the deep space probe needs to be used for detecting the neutron 238 PuO 2 The oxygen 18 in (b) is replaced with oxygen 16.
At present, the relevant technology is generally to put plutonium dioxide and a carrier medium rich in oxygen 16 in a closed container, and to utilize the chemical potential difference between plutonium dioxide and oxygen 18 in the carrier medium under high temperature conditions, so that oxygen 18 in plutonium dioxide diffuses into the carrier medium, and the enrichment of oxygen 16 in plutonium dioxide is realized. The method needs to continuously fill new carrier medium rich in 16 oxygen, so that the method has complex process and high process cost, and the process stability is easily influenced by the surface form of the plutonium dioxide and the feeding amount of the plutonium dioxide.
Disclosure of Invention
In view of the above problems, the present application provides a method for preparing a metal oxide enriched with oxygen 16, which can simplify the process flow and reduce the process cost.
The present application provides a method for preparing an oxygen 16-enriched metal oxide, comprising: preparing a salt solution of the metal using the oxygen 16 enriched water; adding an oxygen 16-enriched oxalic acid solution to the salt solution to obtain an oxygen 16-enriched oxalate precipitate of the metal; the oxalate precipitate is calcined in an oxygen 16-enriched oxygen gas to produce an oxygen 16-enriched metal oxide.
According to the preparation method of the oxygen 16-enriched metal oxide provided by the embodiment of the application, the metal salt solution is prepared by using the oxygen 16-enriched water, the oxygen 16-enriched oxalic acid solution is added into the salt solution to react to obtain the oxygen 16-enriched oxalate precipitate, and finally the oxalate precipitate is placed into the oxygen 16-enriched oxygen to be calcined to obtain the oxygen 16-enriched metal oxide. According to the embodiment of the invention, the oxygen 16-enriched water and the oxygen 16-enriched gas are used as raw materials for preparation through a chemical synthesis method, so that the metal oxide enriched with oxygen 16 can be directly obtained, a process for replacing oxygen 18 in the oxide with oxygen 16 in the related technology is omitted, and the technical effects of simplifying the process flow and reducing the process cost are further achieved.
Drawings
The foregoing and other objects, features and advantages of the application will be apparent from the following description of embodiments of the application with reference to the accompanying drawings in which:
FIG. 1 schematically shows a flow diagram of a method of making an oxygen 16-enriched metal oxide according to an embodiment of the present application.
Detailed Description
Hereinafter, embodiments of the present application will be described with reference to the accompanying drawings. It is to be understood that such description is merely illustrative and not intended to limit the scope of the present application. In the following detailed description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the embodiments of the application. It may be evident, however, that one or more embodiments may be practiced without these specific details. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present application.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The terms "comprises," "comprising," and the like, as used herein, specify the presence of stated features, steps, operations, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, or components.
All terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art unless otherwise defined. It is noted that the terms used herein should be interpreted as having a meaning that is consistent with the context of this specification and should not be interpreted in an idealized or overly formal sense.
In those instances where a convention analogous to "at least one of A, B, and C, etc." is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., "a system having at least one of A, B, and C" would include but not be limited to systems that have A alone, B alone, C alone, A and B together, A and C together, B and C together, and/or A, B, and C together, etc.). In those instances where a convention analogous to "at least one of A, B, or C, etc." is used, in general such a construction is intended in the sense one having skill in the art would understand the convention (e.g., "a system having at least one of A, B, or C" would include but not be limited to systems that have A alone, B alone, C alone, A and B together, A and C together, B and C together, and/or A, B, and C together, etc.).
Plutonium 238 has higher specific heat power (0.4W/g- 238 PuO 2 0.45W/g-Pu, calculated as 80% abundance of plutonium 238), and a long half-life (87.7 years), plutonium 238 replaced the initial source of polonium 210 in the middle of the 20 th century, and gradually became the main representative of nuclear energy for deep space exploration. At the beginning, a static Thermoelectric isotope battery represented by an isotope Thermoelectric Generator (RTG) generally uses plutonium 238 as a radioactive source. However, since metallic plutonium has a low melting point and undergoes spontaneous decay to cause fatigue in a crystal structure, physical properties are deteriorated under high-temperature working conditions, and the service life of the isotope battery is reduced. With the development of material science and preparation technology, the development of the method is gradually advanced 238 PuO 2 A microsphere, 238 PuO 2 Ceramics and 238 PuO 2 -Mo ceramics and the like 238 PuO 2 Chemical formVarious types of core blocks of the formula (I), 238 PuO 2 the pellet material with high melting point, stable irradiation and high safety is used as the new generation of radioactive source for static thermoelectric isotope battery and is widely used so far.
Plutonium 238 isotope batteries are commonly used for deep space exploration. Because the spacecraft used in the deep space exploration process is generally far away from the sun, the spacecraft cannot receive sunlight irradiation or receives weak illumination, the spacecraft is in an extremely low temperature environment and cannot generate electricity by utilizing solar energy, and a detector device in the extremely low temperature environment loses energy supply, cannot work and even can be damaged by low temperature. If use the RHU to keep warm to the spacecraft, can guarantee that the spacecraft lasts work or not damaged by low temperature under low temperature environment, if use the RTG of RHU energy supply, will solve power supply problem and heat supply problem simultaneously.
At present, space nuclear power supplies applied in the world comprise a space stacking plutonium 238 isotope power supply and a temperature difference conversion type plutonium 238 isotope power supply, the space stacking plutonium 238 isotope power supply has high electric output power, and the temperature difference conversion type plutonium 238 isotope power supply has long service life, high reliability, small volume and weight. Therefore, the space stack plutonium 238 isotope power supply is suitable for tasks such as mars and lunar bases, and the temperature difference conversion type plutonium 238 isotope power supply is particularly suitable for deep space exploration tasks due to the advantages of volume and weight.
Plutonium 238 belongs to the alpha decay nuclide, and because of the very short range, alpha particles do not need to be shielded in RTGs, and the neutron and gamma dose rates of plutonium 238 are also very low (where each hundred watts are encapsulated by a metallic sheath) 238 PuO 2 The neutron dose rate at 1m is 0.042mSv/h, the gamma dose rate is 0.008 mSv/h), and the low-power RTG or RHU almost does not need to consider the radiation protection problem. However, high-power plutonium 238 batteries such as those mounted on MMRTG (Multi Mission RTG) and GPHS-RTG (General Purpose heat Source RTG/modular heat Source RTG) 238 PuO 2 The pellets reach 5kg and 10kg grades respectively, and the weight ratio is 0.4W/g- 238 PuO 2 The thermal power of the meter reaches 2KW and 4KW respectively, and the position corresponding to 1m of the meterThe radiation dose rate can reach 1mSv/h and 2mSv/h respectively. The ionizing radiation of the high-power RTG will have great influence on the service life of the deep space detector and the life and health of astronauts.
In order to solve the problem of higher radiation level of high-heat-power plutonium 238 thermal power source, reduction of neutron emissivity of plutonium dioxide has been carried out 238 PuO 2 Study of oxygen 16 substitution technique. Plutonium 238 belongs to alpha decay nuclide, the metal of which has low neutron and gamma dose rates, the neutron comes from spontaneous fission, and the emissivity is 2500-2600 n/s-g 238 Pu。
Due to the fact that 238 PuO 2 The oxygen element in the oxygen-enriched air comes from the nature (air), 238 PuO 2 the composition of medium oxygen is mainly oxygen 16 (99.757%), oxygen 17 (0.038%) and oxygen 18 (0.205%). In that 238 PuO 2 The (alpha, n) reaction threshold energy of the medium oxygen 16 is 15.24MeV, which exceeds the energy of plutonium 238 decay alpha particles by 5.499MeV, so that the (alpha, n) reaction of the oxygen 16 hardly occurs. While the (α, n) reaction threshold energies of oxygen 17 and oxygen 18 are 0MeV and 0.852MeV, respectively, there is a certain probability of generating neutrons by the (α, n) reaction. Wherein the reaction cross sections of the (α, n) reactions of oxygen 17 and oxygen 18 are 206mb and 440mb, respectively. 238 PuO 2 Influenced by the (alpha, n) reaction of alpha particles with oxygen 17 or oxygen 18, 238 PuO 2 the neutron emissivity (the number of neutrons per unit of plutonium 238 generated per unit time) of (1) is high, about 15000 to 19000n/s-g plutonium 238. Since the oxygen 17 content is 0.037%, the oxygen 18 content is 0.204%. Thus, is at 238 PuO 2 In the case of oxygen 16 enrichment, i.e. to produce oxygen 16 enriched 238 PuO 2 Can reduce 238 PuO 2 To a level close to the neutron emissivity of metallic plutonium (n/s-g plutonium 238).
In the related art, the method is generally to 238 PuO 2 Placing in a closed container with a carrier medium rich in oxygen 16, and subjecting to high temperature 238 PuO 2 ( 238 PuO 2 Natural oxygen abundance of oxygen) and oxygen 18 in the oxygen 16 carrier medium, to achieve 238 PuO 2 The intermediate oxygen 18 diffuses toward the oxygen 16 medium. With timeThe movement of the patient can be completed, 238 PuO 2 the oxygen 18 abundance in the medium is continuously decreased and the oxygen 18 abundance of the oxygen 16 carrier medium is increased, and then the oxygen 16 carrier medium is discharged and charged with new oxygen 16 carrier medium to continue the exchange reaction. Through continuous exchange, will eventually 238 PuO 2 To a level close to the oxygen 18 abundance in the oxygen 16 carrier medium, i.e. to a level at which the oxygen 18 abundance in the carrier medium is reduced 238 PuO 2 Medium oxygen 16 enrichment. Depending on the chemical form of the oxygen 16 support medium employed, the oxygen 16 displacement process can be divided into an oxygen 16 water vapor process and an oxygen 16 oxygen displacement process. The replacement process needs to continuously replace the oxygen 16 carrier medium, and has the disadvantages of complex process flow, high process cost and incapability of realizing 238 PuO 2 The accurate quantification of the abundance of intermediate oxygen 16, and the process stability are susceptible to the surface morphology of plutonium dioxide and the amount of plutonium dioxide charged.
In view of this, the present application provides a method for preparing an oxide enriched with oxygen 16, which has a simple process flow and a low process cost. Specifically, the method comprises preparing a salt solution of the metal using oxygen 16 enriched water; adding an oxygen 16-enriched oxalic acid solution to the salt solution to obtain an oxygen 16-enriched oxalate precipitate of the metal; the oxalate precipitate is calcined in an oxygen 16-enriched atmosphere to produce an oxygen 16-enriched metal oxide.
FIG. 1 schematically shows a flow diagram of a method of making an oxygen 16-enriched metal oxide according to an embodiment of the present application.
As shown in fig. 1, the method for preparing the oxygen 16-enriched metal oxide includes operations S101 to S103.
In operation S101, a salt solution of a metal is prepared by enriching water with oxygen 16. Wherein the metal is a third subgroup element.
In operation S102, an oxygen 16-enriched oxalic acid solution is added to the salt solution to obtain an oxygen 16-enriched oxalate precipitate of the metal.
In operation S103, the oxalate precipitate is calcined in an oxygen 16-enriched oxygen gas to obtain an oxygen 16-enriched metal oxide of the metal.
According to the examples of the present application, the metal used may be plutonium or cerium, the oxide finally produced being plutonium dioxide or cerium dioxide enriched with oxygen 16.
According to an embodiment of the present application, in performing operation S101, a nitrate or chloride of a metal may be dissolved in oxygen-16 enriched water to obtain a salt solution. Illustratively, in preparing oxygen 16-enriched ceria, cerium nitrate solution may be formed using oxygen 16-enriched water to dissolve the cerium nitrate. When preparing plutonium dioxide enriched with oxygen 16, plutonium chloride or plutonium nitrate can be selected as the plutonium salt. Illustratively, when plutonium chloride is selected, the plutonium chloride solution can be formed by dissolving plutonium chloride with oxygen 16 enriched water.
In some embodiments, when preparing oxygen 16-enriched plutonium dioxide, metallic plutonium may be dissolved in an oxygen 16-enriched hydrochloric acid solution to form a plutonium salt solution when preparing a plutonium salt solution using oxygen 16-enriched water, wherein the oxygen 16-enriched hydrochloric acid solution is formed by pressurizing oxygen 16-enriched water with hydrogen chloride gas.
In some embodiments, the metal oxide may be dissolved in an oxygen 16-enriched nitric acid solution to form a metal salt solution, wherein the oxygen 16-enriched nitric acid solution is formed by mixing oxygen 16-enriched water with oxygen 16-enriched nitric acid. By way of example, it is also possible to prepare oxygen 16-enriched plutonium dioxide 238 PuO 2 The plutonium nitrate solution is obtained by dissolving the nitric acid solution obtained by mixing the oxygen 16-enriched water and the oxygen 16-enriched nitric acid.
In the preparation of the salt solution, the embodiment of the application removes or minimizes the oxygen 18 in the solution environment by using a solvent such as oxygen 16 enriched water, thereby reducing the abundance of the oxygen 18 in the finally prepared oxide.
In addition, in the production of oxygen 16-enriched plutonium dioxide, it is also possible to concentrate a plutonium nitrate solution in a conventional plutonium production process to obtain a plutonium solution, which participates in the subsequent reaction as a salt solution. The preparation method in the embodiment can be directly connected into the traditional plutonium dioxide preparation process, and the process operation is simple. It is understood that when a salt solution is obtained by concentrating a plutonium nitrate solution in a plutonium production process, nitrate is present as a saltAnd natural abundance oxygen elements are easily introduced into the solution system, and the final preparation can be improved to a certain extent 238 PuO 2 Abundance of medium oxygen 18.
According to an embodiment of the present application, the oxygen 16-enriched oxalic acid solution used in operation S102 may be an oxygen 16-enriched oxalic acid or an oxalic acid solution diluted in oxygen 16-enriched water. The oxalate precipitate enriched in oxygen 16 is plutonium oxalate enriched in oxygen 16 or cerium oxalate enriched in oxygen 16.
When preparing plutonium dioxide, operation S102 may comprise the following operations: the reaction equation for obtaining an oxygen 16-enriched plutonium oxalate precipitate can be shown in equation (1) by adding an oxygen 16-enriched oxalic acid solution to a plutonium salt solution to form an oxygen 16-enriched plutonium oxalate precipitate.
2 238 Pu x+ + x C 2 16 O 4 2- → 238 Pu 2 (C 2 16 O 4 2- ) x ↓ (1)
Wherein, pu x+ Is plutonium ion, C 2 16 O 4 2- Is the ionic oxalate, and the ionic oxalate is the ionic oxalate, 238 Pu 2 (C 2 16 O 4 2- ) x is plutonium oxalate precipitate.
According to an embodiment of the present application, operation S102 may further include the following operations: adding an oxalic acid solution enriched with oxygen 16 into a metal salt solution, and aging for a preset time to obtain a suspension; the suspension was filtered to obtain an oxalate precipitate enriched in oxygen 16. The examples of the present application may allow for the formation of larger particles of oxalate precipitate through the aging process.
According to the embodiment of the present application, when plutonium dioxide is produced, an oxygen 16-enriched oxalic acid solution is added to a plutonium salt solution, an oxygen 16-enriched plutonium oxalate precipitate is formed, at this time, the chemical reaction shown in formula (1) may not be completely reacted, that is, all the oxygen 16-enriched plutonium oxalate precipitate is not obtained, and at this time, the size of the oxygen 16-enriched plutonium oxalate precipitate may be small, so that it is necessary to age the reaction solution for a certain preset time after the plutonium oxalate is completely precipitated to obtain a suspension, for example, 20 to 30min, so as to increase the size of the plutonium oxalate precipitate. After aging for a certain time, the plutonium oxalate precipitate enriched with oxygen 16 in the suspension can be filtered off.
In the filtration of the plutonium oxalate precipitate enriched with oxygen 16, according to the examples of the present application, it is necessary to filter the suspension in a device filled with a protective atmosphere. The protective atmosphere may comprise nitrogen or argon. Specifically, when filtering the suspension, the filtration may be performed in a glove box filled with nitrogen or argon, a hot chamber filled with nitrogen or argon, or the preparation process may be performed in a closed space filled with nitrogen or argon to prevent oxygen in the environment from exchanging with plutonium oxalate and adversely affecting the enrichment of oxygen 16 during the spontaneous heating of plutonium oxalate.
According to an embodiment of the present application, operation S103 may further include the following operations: placing the oxalate precipitate in an atmosphere furnace, wherein the atmosphere in the atmosphere furnace is a protective atmosphere; after the temperature of the atmosphere furnace is raised to a preset temperature, maintaining the atmosphere furnace at the preset temperature; while the atmospheric furnace is maintained at the predetermined temperature, oxygen 16-enriched oxygen is introduced into the atmospheric furnace so that the oxalate precipitate is calcined in the oxygen 16-enriched oxygen to obtain an oxygen 16-enriched metal oxide. In the examples of the present application, the oxalate is decomposed to form a metal oxide by calcining the oxalate in oxygen 16-enriched oxygen, and carbon in the solid product obtained by the decomposition is removed by oxygen, wherein the carbon in the solid product is removed by forming carbon dioxide or carbon monoxide in the oxygen at a high temperature.
After the oxalate precipitate is placed in the atmosphere furnace, the atmosphere furnace can be subjected to multiple times of gas washing operation, and protective atmosphere is introduced into the atmosphere furnace. Specifically, the atmosphere furnace may be vacuumized to remove the impurity gas in the furnace, and then argon gas may be introduced into the atmosphere furnace as a protective atmosphere to achieve a gas washing operation of the atmosphere furnace. The operations of vacuumizing and argon introducing can be repeatedly carried out for a plurality of times so as to realize a plurality of times of gas washing of the atmosphere furnace.
According to embodiments of the present application, the oxygen 16-enriched metal oxide may be oxygen 16-enriched plutonium dioxide or oxygen 16-enriched ceria. When preparing plutonium dioxide, operation S103 may also be understood as putting the oxygen 16-enriched plutonium oxalate cake (composed of the filtered oxygen 16-enriched plutonium oxalate) into an atmosphere furnace, evacuating the atmosphere furnace to remove impurity gases, then introducing argon gas into the atmosphere furnace, and repeating the operations of evacuating and introducing argon gas several times to achieve purging of the atmosphere furnace.
After the gas washing is finished, argon can be introduced again, and the atmosphere furnace is heated to the preset temperature. The preset temperature may be greater than or equal to 600 c in this embodiment. After the temperature is kept for a certain time at the preset temperature, oxygen enriched with oxygen 16 is introduced to react with the oxalic plutonium enriched with oxygen 16, and the plutonium dioxide enriched with oxygen 16 is obtained. After the reaction is completed, the carbide in the reaction product can be removed by a common gas treatment method. The reaction equation between the oxygen 16-enriched plutonium oxalate and the oxygen 16-enriched oxygen gas can be shown in equation (2).
238 Pu 2 (C 2 16 O 4 2- ) x +2 16 O 2→ 2 238 Pu 16 O 2 +2x CO 2 * (2)
Wherein the content of the first and second substances, 238 Pu 2 (C 2 16 O 4 2- ) x in order to precipitate the plutonium oxalate, 16 O 2 oxygen gas enriched with the oxygen 16, 238 Pu 16 O 2 plutonium dioxide, CO enriched with oxygen 16 2 The carbon dioxide, i.e. the carbides formed by the reaction, * it can be shown that the carbide formed may also be CO.
According to embodiments of the present application, after calcination, the oxygen 16-enriched metal oxide can be stored in a closed, oxygen-free metal can and the metal can is subjected to a temperature-reducing heat-dissipating process.
According to the embodiment of the present application, the produced plutonium dioxide powder particles enriched with oxygen 16 need to be stored in a closed, oxygen-free heat-resistant metal can, and a cooling and heat dissipation process needs to be performed for a single heat-resistant metal can in which a large number of plutonium dioxide particles are stored. If plutonium dioxide powder particles enriched with oxygen 16 are not stored in a closed, oxygen-free environment, when plutonium dioxide enriched with oxygen 16 comes into contact with oxygen in the environment, the plutonium dioxide is easily subjected to oxygen isotope exchange with ambient oxygen again under self-heating, so that the abundance of oxygen 18 per se is increased, which is not favorable for oxygen 16 enrichment.
In the examples of the present application, plutonium dioxide powder enriched with oxygen 16 is obtained by enriching oxalic acid with plutonium solution and oxygen 16 by chemical synthesis, synthesizing plutonium oxalate enriched with oxygen 16 under conditions in which oxygen 18 in the solution environment is removed or oxygen 18 in the solution environment is minimized, and then by high-temperature calcination in an environment of oxygen 16-enriched oxygen gas. Since the oxygen 16-enriched plutonium dioxide obtained from a plutonium dioxide-enriched solution of oxygen 16 and oxygen 16-enriched oxygen is used, the abundance of oxygen 16 and oxygen 18 in plutonium dioxide should be the same as the abundance of oxygen 16 and oxygen 18 in the raw material, respectively, and since the abundance of oxygen 16 in the raw material can be measured and controlled, and thus the abundance of oxygen 16 in plutonium dioxide can be controlled, accurate quantification of the abundance of oxygen 16 in plutonium dioxide can be achieved.
According to the preparation method of the oxygen 16-enriched metal oxide provided by the embodiment of the application, the salt solution of the metal is prepared by using the oxygen 16-enriched solution, the oxygen 16-enriched oxalic acid solution is added into the salt solution to obtain the oxygen 16-enriched oxalate precipitate, and then the oxalate precipitate is placed into the oxygen 16-enriched oxygen for calcination to obtain the oxygen 16-enriched metal oxide. Because the preparation is carried out by using the oxygen 16-enriched salt solution and the oxygen 16-enriched atmosphere as raw materials, the metal oxide enriched with oxygen 16 can be directly obtained, the process of replacing oxygen 18 in the dioxide with oxygen 16 in the related technology is omitted, and the technical effects of simplifying the process flow and reducing the process cost are achieved.
Example 1
First is the acquisition of the plutonium solution. The plutonium salt is preferably plutonium chloride. Plutonium chloride is dissolved in water enriched with oxygen 16 to form a plutonium solution. Metallic plutonium may also be selected, and the plutonium solution may be obtained by dissolving the metallic plutonium in hydrochloric acid (formed by pressurizing water enriched with oxygen 16 with HCl). A plutonium solution can also be obtained by dissolving plutonium dioxide in water enriched with oxygen 16 and nitric acid enriched with oxygen 16. The plutonium nitrate solution can also be concentrated in the plutonium preparation process to obtain a plutonium solution. When the plutonium solution is obtained by a method of concentrating a plutonium nitrate solution in a plutonium preparation process, natural abundance oxygen elements are easily introduced into a nitrate radical and solution system, so that the abundance of oxygen 18 in the later plutonium dioxide preparation process can be improved.
After the plutonium solution has been prepared, an oxalic acid solution enriched in oxygen 16 can be added to the plutonium solution to form an oxygen 16-enriched plutonium oxalate precipitate. And aging the suspension for more than 20min after the plutonium oxalate enriched in oxygen 16 is completely precipitated so as to increase plutonium oxalate particles. The plutonium oxalate solids enriched in oxygen 16 or the plutonium oxalate cake enriched in oxygen 16 can be obtained by filtration after aging. The process of obtaining the plutonium oxalate filter cake is carried out in a nitrogen or argon filled glove box or a hot chamber or in a closed space protected by nitrogen or argon, so that the exchange reaction between environmental oxygen and plutonium oxalate in the self-heating process of plutonium oxalate is prevented.
After obtaining the plutonium oxalate filter cake that oxygen 16 is enriched, can put into the atmosphere stove with oxygen 16 enriched plutonium oxalate filter cake, carry out the evacuation degasification to the atmosphere stove, then let in argon gas, the operation of carrying out the evacuation more than the cubic and letting in argon gas repeatedly to wash gas to the atmosphere stove. And introducing argon gas after the gas washing, rapidly raising the temperature in the atmosphere furnace to be more than or equal to 600 ℃, preserving the heat for 1-2 h, and continuously introducing oxygen enriched with oxygen 16 for 1-2 h after preserving the heat for 1-2 h so that the oxygen enriched with oxygen 16 and the plutonium oxalate enriched with oxygen 16 react to obtain plutonium dioxide enriched with oxygen 16.
The abundance of oxygen 16 in plutonium dioxide can be measured after obtaining oxygen 16 enriched plutonium dioxide, or alternatively the abundance of oxygen 18 in plutonium dioxide. Since an oxygen 16-enriched solution and oxygen 16-enriched oxygen gas are used as the oxygen 16-enriched plutonium dioxide produced from the raw material, the abundance of oxygen 16 and oxygen 18 in plutonium dioxide should be the same as the abundance of oxygen 16 and oxygen 18 in the raw material, respectively.
The obtained oxygen 16-enriched plutonium dioxide powder needs to be stored in a sealed, oxygen-free heat-resistant metal can, and the temperature reduction and heat dissipation treatment needs to be performed for a single heat-resistant metal can in which a large number of plutonium dioxide powders are stored. Unless oxygen 16-enriched plutonium dioxide powder is stored in a closed, oxygen-free environment, oxygen 16-enriched plutonium dioxide, upon exposure to ambient oxygen, is susceptible to oxygen isotope exchange with ambient oxygen under self-heating conditions, resulting in an increase in the abundance of native oxygen 18.
Example 2
In accordance with embodiments of the present application, a method for producing oxygen 16-enriched ceria is also provided, as cerium and plutonium are located in the same subgroup, with adjacent periods, and are chemically similar and more reactive.
Firstly, cerium solution is prepared, cerium nitrate can be used as cerium salt, and the cerium nitrate is dissolved by oxygen 16 enriched water to obtain the cerium nitrate solution. Wherein the gram number of cerium nitrate may be 8g to 100g, for example 8g, 10g, 20g, 30g, 40g, 50g, 60g, 70g, 80g, 90g, 100g, etc., and the volume of oxygen 16-enriched water may be 10ml to 100ml, for example 10ml, 20ml, 30ml, 40ml, 50ml, 60ml, 70ml, 80ml, 90ml, 100ml, etc. The gram number of cerium nitrate and the volume of oxygen 16-enriched water may be adjusted adaptively according to actual needs, but it should be noted that if the gram number or the volume of cerium nitrate and the volume of oxygen 16-enriched water are too small, the difficulty of operation may be increased, and if the gram number and the volume are too small or the gram number and the volume are too small, the collection rate of cerium oxide may be decreased.
The cerium oxalate precipitate can be prepared after the cerium solution is prepared. The oxygen 16-enriched oxalic acid solution can be added to the cerium nitrate solution to form a plutonium oxalate precipitate. After the cerium nitrate is completely precipitated, aging the solution for 20-30 min at 40-50 ℃, and filtering the aged suspension to obtain the oxygen 16-enriched cerium oxalate solid precipitate. The aging time and the aging temperature can be adaptively adjusted according to actual needs.
After filtering the cerium oxalate precipitate, a wet cake of cerium oxalate can be obtained. And putting the oxygen-16-enriched cerium oxalate wet cake into an atmosphere furnace, vacuumizing and degassing the atmosphere furnace, introducing argon, and repeatedly vacuumizing for more than three times and introducing the argon so as to carry out gas washing on the atmosphere furnace. And after gas washing, introducing argon, rapidly raising the temperature in the atmosphere furnace to be more than or equal to 600 ℃, preserving the temperature for 1-2 h, and continuously introducing oxygen 16-enriched oxygen for 1-2 h after preserving the temperature for 1-2 h so that the oxygen 16-enriched oxygen reacts with the oxygen 16-enriched cerium oxalate to obtain the oxygen 16-enriched cerium dioxide.
The abundance of oxygen 16 in ceria can be detected after obtaining oxygen 16-enriched ceria, or alternatively, the abundance of oxygen 18 in ceria can be detected. Since oxygen 16-enriched ceria prepared by using an oxygen 16-enriched solution and oxygen 16-enriched oxygen as raw materials is used, the abundance of oxygen 16 and oxygen 18 in ceria should be the same as the abundance of oxygen 16 and oxygen 18 in the raw materials, respectively. In the embodiment of the application, the abundance of oxygen 18 in the oxalic acid solution enriched with oxygen 16 is 3 percent, the abundance of oxygen 18 in the obtained cerium oxide enriched with oxygen 16 is slightly increased because of the influence of nitrate (natural oxygen abundance) in the solution, and the abundance of oxygen 18 is 3 percent to 6 percent as determined by mass spectrometry. The experimental conditions corresponding to the abundance of the oxygen 18 can be that 8g of cerous nitrate, 50ml of water enriched with the oxygen 16 and oxalic acid solution enriched with the oxygen 16 are added to form cerous oxalate precipitate, the precipitate is aged for 20min at the temperature of 40-50 ℃, the temperature in an atmosphere furnace is quickly raised to be more than or equal to 600 ℃, the temperature is kept for 1h, oxygen enriched with the oxygen 16 is continuously introduced for 1h after the temperature is kept for 1h, and the calcination is carried out.
The obtained oxygen 16-enriched cerium oxide powder needs to be stored in a sealed, oxygen-free heat-resistant metal can, and the temperature reduction and heat dissipation treatment is required for the single heat-resistant metal can which is stored more. Without storing the oxygen 16-enriched ceria powder in a closed, oxygen-free environment, the oxygen 16-enriched ceria, upon contact with ambient oxygen, tends to cause the ceria to undergo oxygen isotope exchange with ambient oxygen again under self-heating conditions, resulting in an increase in the abundance of native oxygen 18.
According to the examples of the present application, oxygen 16-enriched cerium oxalate is synthesized by enriching oxalic acid with a cerium solution and oxygen 16 by using a chemical synthesis method under the condition of removing oxygen 18 in the solution environment or minimizing oxygen 18 in the solution environment, and then oxygen 16-enriched cerium oxide powder is obtained by high-temperature calcination in the environment of oxygen 16-enriched oxygen. Because the oxygen 16-enriched ceria prepared by using the oxygen 16-enriched solution and the oxygen 16-enriched oxygen as raw materials is used, the abundance of the oxygen 16 and the oxygen 18 in the ceria should be the same as the abundance of the oxygen 16 and the oxygen 18 in the raw materials, respectively, and the abundance of the oxygen 16 in the raw materials can be measured and controlled, and further the abundance of the oxygen 16 in the ceria can be controlled, so that the abundance of the oxygen 16 in the ceria can be accurately quantified.
It should be noted that, unless explicitly stated that there is an execution sequence between different operations or there is an execution sequence between different operations in technical implementation, the execution sequence between multiple operations may not be sequential, or multiple operations may be executed simultaneously in the flowchart in this disclosure.
It will be appreciated by a person skilled in the art that various combinations and/or combinations of features described in the various embodiments and/or claims of the present application are possible, even if such combinations or combinations are not explicitly described in the present application. In particular, various combinations and/or combinations of the features recited in the various embodiments and/or claims of the present application may be made without departing from the spirit and teachings of the present application. All such combinations and/or associations are intended to fall within the scope of this application.
The embodiments of the present application are described above. However, these examples are for illustrative purposes only and are not intended to limit the scope of the present application. Although the embodiments are described separately above, this does not mean that the measures in the embodiments cannot be used advantageously in combination. The scope of the application is defined by the appended claims and equivalents thereof. Various alternatives and modifications can be devised by those skilled in the art without departing from the scope of the present application, and these alternatives and modifications are intended to fall within the scope of the present application.
Claims (10)
1. A method for producing an oxygen 16-enriched metal oxide, comprising:
preparing a salt solution of the metal using the oxygen 16 enriched water; wherein the metal is a third subgroup element;
adding an oxygen 16-enriched oxalic acid solution to the salt solution to obtain an oxygen 16-enriched oxalate precipitate of the metal;
calcining the oxalate precipitate in oxygen 16 enriched oxygen to obtain the oxygen 16 enriched metal oxide.
2. The method of claim 1, wherein the metal is plutonium or cerium.
3. The method of claim 2, wherein the preparing a salt solution of a metal using oxygen 16 enriched water comprises:
and dissolving nitrate or chloride of the metal into oxygen-16 enriched water to obtain the salt solution.
4. The method of claim 2, wherein said preparing a salt solution of a metal using oxygen 16 enriched water comprises:
the metal oxide is dissolved in an oxygen 16-enriched nitric acid solution obtained by mixing oxygen 16-enriched water with oxygen 16-enriched nitric acid.
5. The method of claim 2, wherein the metal is plutonium; the preparation of a salt solution of a metal using oxygen 16 enriched water comprises:
metallic plutonium is dissolved in a hydrochloric acid solution enriched in oxygen 16, which is formed by pressurizing oxygen 16-enriched water with hydrogen chloride gas.
6. The method of claim 1, wherein the adding the oxygen 16-enriched oxalic acid solution to the salt solution to obtain the oxygen 16-enriched oxalate precipitate of the metal comprises:
adding the oxalic acid solution enriched with the oxygen 16 into the salt solution, and then aging for a preset time to obtain a suspension;
filtering the suspension to obtain the oxalate precipitate enriched in oxygen 16.
7. The method of claim 6, wherein the filtering the suspension comprises:
the suspension was filtered in an apparatus filled with a protective atmosphere.
8. The method of claim 7, wherein the subjecting the oxalate precipitate to calcination in oxygen 16-enriched oxygen to produce the oxygen 16-enriched metal oxide comprises:
placing the oxalate precipitate in an atmosphere furnace, wherein the atmosphere in the atmosphere furnace is the protective atmosphere;
after the temperature of the atmosphere furnace is increased to a preset temperature, maintaining the atmosphere furnace at the preset temperature;
and introducing the oxygen 16-enriched oxygen gas into the atmosphere furnace while the atmosphere furnace is maintained at the preset temperature, so that the oxalate precipitate is calcined in the oxygen 16-enriched oxygen gas to obtain the oxygen 16-enriched metal oxide.
9. The method of claim 8, further comprising:
and after the oxalate precipitate is placed in the atmosphere furnace, carrying out multiple times of gas washing operation in the atmosphere furnace, and introducing the protective atmosphere into the atmosphere furnace.
10. The method of claim 1, further comprising:
storing the oxygen 16-enriched metal oxide in a closed, oxygen-free metal can;
and cooling and radiating the metal tank.
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