A method of coupling production of boron isotopes

Abstract

This application provides a method for coupled production of boron isotopes, belonging to the field of boron isotope manufacturing technology. The method for coupled production of boron isotopes includes the following steps: a first-stage enrichment of naturally abundant BF3 using a chemical exchange method to obtain a boron isotope intermediate; the boron isotope intermediate contains… 10 The abundance of boron isotopes is 50%–85%; a second-stage enrichment of boron isotope intermediates is carried out using a low-temperature distillation method until… 10 The abundance of B isotopes is not less than 96%. This method can effectively solve the engineering problems of implementing isotope cryogenic distillation. It also has the synergistic advantages of chemical exchange method (short time, low engineering difficulty) and cryogenic distillation method (simple process, no side reactions, and high product purity).

Description

Technical Field

[0001] This application relates to the field of boron isotope manufacturing technology, and more specifically, to a method for coupling the production of boron isotopes. Background Technology

[0002] Boron exists in nature in two stable isotopes ( 10 B and 11 B), with natural abundances of approximately 19.8% and 80.2%, respectively. Among these, high purity and high abundance... 10 Boron-10 (B-10) with a thermal neutron capture cross-section of 3835 bp is widely used in key areas such as nuclear reactor control rods, nuclear protection materials, and neutron capture therapy for cancer (BNCT, where boron-10 enrichment must exceed 99%). High purity and high abundance are also important applications. 11 Boron (B), as a P-type doping source in semiconductors, plays an irreplaceable role in the ion implantation process of integrated circuit manufacturing. With the rapid development of my country's nuclear power industry and the accelerating pace of domestic production of high-end chips, there is an increasingly urgent need for a large-scale and stable supply of high-abundance boron isotopes.

[0003] Currently, the main methods for boron isotope separation in industrial production are chemical exchange and cryogenic distillation. While chemical exchange can operate at atmospheric pressure, it suffers from low yield, high toxicity of the complexing agent, and severe equipment corrosion, especially in high-abundance regions (abundance exceeding 80%), due to the presence of... 10 When boron trifluoride (B) concentration approaches equilibrium, the reflux ratio must be significantly increased (typically exceeding 200) to continue driving the exchange reaction towards enrichment, leading to a sharp increase in equipment investment and energy consumption. Simultaneously, the thermal cracking of the boron trifluoride-anisole complex produces certain side reactions, resulting in decreased anisole purity and reduced separation efficiency. Cryogenic distillation, due to its advantages of simple process and high product purity and abundance, is widely used in the manufacturing of electronic specialty gases and is becoming a research hotspot in isotope separation and purification. However, since the separation principle of cryogenic distillation utilizes the slight difference in saturated vapor pressure between isotope molecules to achieve separation... 10 B and 11 Taking B as an example, under normal pressure, the separation factor between the two is only 1.006~1.008, and the relative volatility of the two isotopes is as low as 1.006, which makes the theoretical number of plates required for the low-temperature distillation column as high as thousands, and the height of the distillation column exceeds 100 meters.

[0004] Such extremely tall distillation columns present numerous inherent technical obstacles to the industrial application of cryogenic distillation, severely restricting their large-scale promotion. The core drawback lies in the fact that ultra-high and low temperature distillation columns are extremely sensitive to wind loads, uneven foundation settlement, and external thermal disturbances. To maintain the ultra-steady environment of temperature and pressure within the column, it is usually necessary to construct them using underground deep wells. However, underground deep wells are not only difficult to construct, have long construction periods, and are very expensive, but also present challenges in daily operation and maintenance. Maintenance work is severely limited by space constraints, and once a malfunction occurs, it is often impossible to repair, forcing the equipment to be scrapped, greatly reducing the project's economic viability and feasibility. Currently, in order to alleviate the above-mentioned problems, multi-stage cascade technology is commonly used in engineering. Although this solution can alleviate the engineering implementation problems of ultra-high towers to a certain extent, it has given rise to a series of new contradictions. The core problems include: a significant increase in the number of system pipelines and heat exchange equipment, a sharp increase in the complexity of the process flow diagram, a multiplied increase in the time required for the entire unit to go from start-up to steady-state operation, an increase in the space used for civil engineering, and a significant increase in the total investment scale and operation and maintenance difficulty. It cannot fundamentally solve the inherent engineering bottlenecks of cryogenic distillation.

[0005] In conclusion, there is an urgent need to explore and develop new technological approaches to overcome the engineering limitations of existing cryogenic distillation methods in the field of isotope separation and to meet the pressing requirements of industrial upgrading. Summary of the Invention

[0006] The purpose of this application is to provide a method for coupled production of boron isotopes, which can effectively solve the engineering problems existing in the implementation of isotope low-temperature distillation, and also has the synergistic advantages of chemical exchange method (short time, low engineering difficulty) and low-temperature distillation method (simple process, no side reactions, and high product purity).

[0007] The embodiments of this application are implemented as follows: In a first aspect, embodiments of this application provide a method for coupled production of boron isotopes, comprising the following steps: performing a first-stage enrichment of naturally abundant BF3 using a chemical exchange method to obtain a boron isotope intermediate, wherein the boron isotope intermediate contains... 10 The abundance of boron isotopes is 50%–85%; a second-stage enrichment of boron isotope intermediates is carried out using a low-temperature distillation method until… 10 The abundance of B isotopes is not less than 96%.

[0008] In the above technical solution, the naturally abundant BF3 is first enriched using a chemical exchange method in the first stage, so as to... 10 The abundance of boron isotopes was enriched to 50%–85%, and then cryogenic distillation was used to further enrich the boron isotopes. 10 The boron isotope intermediate, with a significantly higher B isotope abundance than the naturally occurring BF3, underwent a second-stage enrichment until... 10The abundance of B isotopes is not less than 96%. Compared to existing technologies that directly enrich naturally abundant BF3 using cryogenic distillation, this method... 10 The abundance of boron isotopes is no less than 96% (requiring thousands of theoretical plates in the cryogenic distillation column, with a column height exceeding 100 meters), due to the initial feed gas entering the cryogenic distillation column... 10 The abundance of boron isotopes is significantly increased, which can effectively reduce the height of the required cryogenic distillation column, allowing the cryogenic distillation column to be deployed industrially directly in conventional plants (i.e., without the need for deep well technology to install and construct the cryogenic distillation column), thus effectively solving the engineering challenges of implementing isotope cryogenic distillation. At the same time, this application directly uses the chemical exchange method, which is currently industrialized and has a very mature preparation system (compared to cryogenic distillation, it requires significantly less time, and the construction of the required exchange column does not require deep well technology) to assist cryogenic distillation in production, which also has the advantages of being easy to industrialize and requiring a significant reduction in time. Correspondingly, since the entire production process relies on the chemical exchange method and cryogenic distillation to be completed in stages, the entire production process also has the synergistic advantages of the chemical exchange method (short time, low engineering difficulty) and the cryogenic distillation method (simple process, no side reactions, and high product purity).

[0009] In some alternative implementations, the boron isotope intermediate... 10 The abundance of B isotopes is 60%–80%.

[0010] In the above technical solution, the boron isotope intermediate is... 10 The abundance of B isotopes is limited to the above range, which ensures that the initial feed gas entering the cryogenic distillation column... 10 The lower limit of boron isotope abundance has been further increased, thereby more effectively reducing the required height of cryogenic distillation columns. This allows for easier industrial deployment of cryogenic distillation columns in conventional plants, thus more effectively solving the engineering challenges of implementing isotope cryogenic distillation and correspondingly reducing costs. Simultaneously, the boron isotope intermediates... 10 The abundance upper limit of boron isotopes is limited to the above range. Since the increase in abundance per unit tray of the exchange tower is relatively high within this range, fewer exchange tower stages and a lower single tower height are required during the first stage enrichment using the chemical exchange method. Consequently, the preparation cost required for the first enrichment stage is lower and the preparation efficiency is higher. This allows the overall production cost of boron isotopes to be controlled at a low level while maintaining a high production efficiency, so that both stages can operate stably and efficiently within their respective optimal economic zones.

[0011] In some alternative implementations, the isotopic intermediates 10 The abundance of B isotopes is 65%–75%.

[0012] In the above technical solution, the boron isotope intermediate is... 10 The abundance of B isotopes is further limited to the aforementioned range, enabling both stages to operate stably and efficiently within their respective optimal economic zones. A detailed analysis follows: (1) Chemical exchange method has the highest abundance contribution increment per unit tray within this abundance range, and the equipment utilization rate and energy consumption ratio are optimal, compared to directly exchanging natural abundance through chemical exchange method. 10 B isotopes are enriched to an abundance of not less than 96%. In the embodiments of this application, only the naturally abundant isotopes are enriched. 10 When boron isotopes are enriched to a level not exceeding 75%, the number of theoretical plates required for chemical exchange towers is only about 30% of that of the former method, and the number of chemical exchange tower stages is reduced from 6-18 stages to 1-3 stages. The difficulty of multi-tower coordination and side reactions are significantly reduced, and the production capacity is increased by at least 80%. At the same time, when using chemical exchange for enrichment in a low-abundance range with a large material throughput, since it does not need to maintain stable operation at -110℃ to -90℃ as in cryogenic distillation, the unit product energy consumption of chemical exchange enrichment can be reduced by 30% to 40% compared to cryogenic distillation in the process of enriching the same amount of material to the same abundance.

[0013] (2) Low-temperature distillation method from an abundance of not less than 65% 10 B isotopes are enriched at high abundance in the target area, compared to directly refining naturally abundant B isotopes through cryogenic distillation. 10 With boron isotope enrichment reaching an abundance of no less than 96%, the theoretical number of trays in the cryogenic distillation section is reduced from thousands to hundreds, and the total height of the column is correspondingly reduced from hundreds of meters to tens of meters. This allows for industrial deployment within conventional plant buildings, completely eliminating the inherent drawbacks of deep underground wells and ultra-high column operation. At the same time, starting from an abundance of 65% and moving towards higher abundances, the purity and process simplicity advantages of cryogenic distillation in the high-abundance section can be fully utilized. Furthermore, since the chemical exchange method does not participate in the enrichment process in the high-abundance section, it can effectively avoid the core drawbacks of the chemical exchange method in the high-abundance section, such as the surge in reflux ratio and the decline in marginal efficiency caused by equilibrium limitations.

[0014] (3) According to the above-mentioned scientific segmented process, the total cost of the combined production process is only 30% to 40% of that of the single chemical exchange process and only 20% to 30% of that of the single low temperature distillation process. This huge economic effect is not a simple series connection of the two preparation processes, but rather a scientific division of labor between the chemical exchange method and the low temperature distillation method in their respective optimal economic zones, so as to generate comprehensive benefits far exceeding those of their independent operation.

[0015] In some optional embodiments, the first-stage enrichment of naturally abundant BF3 using chemical exchange includes: sequentially performing complexation treatment, chemical exchange treatment, pyrolysis separation treatment, and purification treatment on naturally abundant BF3 and an organic complexing agent; wherein, in the chemical exchange treatment step, the total number of theoretical plates in the chemical exchange column is 100 to 300, and the reflux ratio is 50 to 200; and / or, in the pyrolysis separation treatment step, the pyrolysis separation temperature is 80°C to 220°C.

[0016] In the above technical solution, when the enrichment target of the first stage is 65%~75%, specifically limiting the total theoretical plate number and reflux ratio in the chemical exchange step within this range allows for precise matching of the enrichment target, eliminating plate redundancy and reducing unnecessary energy waste. Simultaneously, it ensures the exchange reaction proceeds fully, yielding reaction products with minimal abundance fluctuations and high purity, reducing the difficulty of subsequent separation and purification. Furthermore, when the enrichment target of the first stage is 65%~75%, specifically limiting the pyrolysis separation temperature within this range allows for the complete decomposition of the complex between BF3 and the organic complexing agent, leaving no unpyrolyzed complex residue, thereby improving the purity of the product in this stage. This pyrolysis temperature can also precisely match the operating conditions of the upstream chemical exchange column, ensuring a stable output of the 65%~75% target enrichment without significant abundance fluctuations.

[0017] In some alternative implementations, the chemical exchange treatment step involves a top temperature of 50°C to 100°C, a bottom temperature of 60°C to 120°C, and a reaction pressure of 0.08 MPa to 0.3 MPa.

[0018] In the above technical solution, when the enrichment target of the first stage is 65%~75% and the total theoretical plate number and reflux ratio of the chemical exchange tower are within a specific range, the top temperature, bottom temperature and reaction pressure of the chemical exchange tower are specifically limited within the above range. This allows the chemical exchange reaction between BF3 and the organic complexing agent to maintain high efficiency and high stability. At the same time, it also makes the temperature, pressure and the total theoretical plate number and reflux ratio highly matched, thereby stably and efficiently outputting the reaction product with the target abundance.

[0019] In some alternative implementations, the step of first-stage enrichment of naturally abundant BF3 using chemical exchange further includes: cooling the organic complexing agent generated in the pyrolysis and separation step, and then conveying the cooled organic complexing agent to a complexing tower in the complexing step for complexing treatment.

[0020] In the above technical solution, the organic complexing agent generated in the pyrolysis and separation step is transported to the complexing tower in the complexing treatment step after cooling for complexing treatment. This can realize the closed-loop process of the organic complexing agent, reduce the amount of fresh organic complexing agent to be replenished, and significantly reduce the cost of raw materials. In particular, cooling the organic complexing agent after high-temperature pyrolysis to the appropriate temperature range of the complexing reaction and then reusing it can maintain the temperature stability in the complexing tower, thereby ensuring the complexing stability and complexing efficiency.

[0021] In some alternative embodiments, the organic complexing agent is selected from at least one of dimethyl ether, diethyl ether, anisole, and methyl isobutyl ketone.

[0022] In the above technical solutions, there are many types of organic complexing agents that can be applied, which can provide a variety of feasible solutions, thus making it easy to make adaptive adjustments to the type of organic complexing agent used according to the actual production line conditions.

[0023] In some alternative implementations, the organic complexing agent is selected from anisole.

[0024] In the above technical solution, the organic complexing agent is selected from anisole. Anisole can react efficiently with BF3 to form a stable complex, and the separation coefficient of the complex formed by the two is large, which can efficiently separate the boron isotope intermediate with the target abundance. At the same time, anisole also has the advantages of good chemical stability, no strong corrosiveness, low requirements for equipment materials and no need for special anti-corrosion materials.

[0025] In some alternative implementations, in the step of second-stage enrichment of boron isotope intermediates using cryogenic distillation, the total theoretical number of theoretical plates in the cryogenic distillation column is 400 to 600, and the reflux ratio is 50 to 300.

[0026] In the above technical solution, when the abundance of the feed gas entering the cryogenic distillation column is within the range of 65% to 75%, the total theoretical number of trays and the reflux ratio of the cryogenic distillation column are specifically limited within this range, which can efficiently and stably generate feed gas with an abundance of not less than 96%. 10 B isotope products; at the same time, the height of the cryogenic distillation column under this process parameter design can be reduced to less than 50 meters, avoiding the inherent defects of high columns being sensitive to wind loads and thermal disturbances. The construction and operation and maintenance costs are reduced by more than 50% compared with the traditional full-process cryogenic distillation process, and the process production cycle under this parameter design can be reduced to 1 to 3 months, which is far lower than the production cycle of several years of the full-process cryogenic distillation process.

[0027] In some alternative implementations, the cryogenic distillation column has a top pressure of 0.08 MPa to 0.5 MPa and a top temperature of -110°C to -90°C.

[0028] In the above technical solution, when the abundance of the feed gas entering the cryogenic distillation column is 65%~75% and the total theoretical plate number and reflux ratio of the cryogenic distillation column are both within a specific range, the top pressure and top temperature of the cryogenic distillation column are specifically limited within the above range. This allows the pressure and temperature to be highly matched with the total theoretical plate number and reflux ratio, thereby stably and efficiently generating the target product with an abundance of not less than 96%.

[0029] In some alternative implementations, the step of second-stage enrichment of boron isotope intermediates using cryogenic distillation further includes: heating the byproduct generated at the top of the cryogenic distillation column, and then conveying the heated byproduct to a chemical exchange column in the chemical exchange treatment step for chemical exchange treatment.

[0030] In the above technical solution, the byproducts generated at the top of the low-temperature distillation column ( 10 B (with an abundance typically not less than 50%) is fed into the chemical exchange column after heating for chemical exchange treatment. This enables a closed-loop process for the byproducts generated in the cryogenic distillation column, reducing material waste and thus lowering production costs. Furthermore, reheating and reusing the byproducts generated in the cryogenic distillation column maintains temperature stability within the chemical exchange column, ensuring the stability and efficiency of the chemical exchange treatment. In particular, the byproducts fed back into the chemical exchange column... 10 The abundance of boron is typically no less than 50%, which is much higher than the natural abundance found in chemical exchange towers. 10 B (around 20%) can significantly reduce the separation load in subsequent processes, thereby reducing the overall production energy consumption of the first enrichment stage by more than 30%. Attached Figure Description

[0031] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0032] Figure 1 A process flow diagram of a method for coupling the production of boron isotopes provided in this application embodiment; Figure 2 A schematic diagram of a production system for coupling the production of boron isotopes is provided in an embodiment of this application; Figure 3 A schematic diagram of a cascaded structure of a chemical exchange tower provided in an embodiment of this application; Figure 4 This is a schematic diagram of a series structure of a cryogenic distillation column provided in an embodiment of this application.

[0033] Icons: 10 - Production system for coupling boron isotope production; 100 - Complexation tower; 200 - Chemical exchange tower; 210 - Chemical exchange sub-tower; 300 - Cracking tower; 400 - Heavy removal distillation tower; 500 - Light removal distillation tower; 600 - Low temperature distillation tower; 610 - Low temperature distillation sub-tower. Detailed Implementation

[0034] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0035] It should be noted that the terms "and / or" in this application, such as "feature 1 and / or feature 2", all refer to the three cases of "feature 1" alone, "feature 2" alone, and "feature 1" plus "feature 2".

[0036] In addition, in the description of this application, unless otherwise stated, "one or more" means two or more; the range of "numerical value a to numerical value b" includes the two endpoints "a" and "b"; and "unit of measurement" in "numerical value a to numerical value b + unit of measurement" represents the "unit of measurement" of both "numerical value a" and "numerical value b".

[0037] The following is a detailed description of a method for coupling and producing boron isotopes according to an embodiment of this application.

[0038] In a first aspect, embodiments of this application provide a method for coupled production of boron isotopes, comprising the following steps: performing a first-stage enrichment of naturally abundant BF3 using a chemical exchange method to obtain a boron isotope intermediate, wherein the boron isotope intermediate contains... 10 The abundance of boron isotopes is 50%–85% (e.g., but not limited to any one of the abundances of 50%, 60%, 70%, 80%, and 85%, or any range between two); a second-stage enrichment of boron isotope intermediates is carried out using cryogenic distillation until… 10 The abundance of B isotopes is not less than 96%.

[0039] In this application, a first-stage enrichment of naturally abundant BF3 is performed using a chemical exchange method to... 10 The abundance of boron isotopes was enriched to 50%–85%, and then cryogenic distillation was used to further enrich the boron isotopes. 10 The boron isotope intermediate, with a significantly higher B isotope abundance than the naturally occurring BF3, underwent a second-stage enrichment until... 10The abundance of B isotopes is not less than 96%. Compared to existing technologies that directly enrich naturally abundant BF3 using cryogenic distillation, this method... 10 The abundance of boron isotopes is no less than 96% (requiring thousands of theoretical plates in the cryogenic distillation column, with a column height exceeding 100 meters), due to the initial feed gas entering the cryogenic distillation column... 10 The abundance of boron isotopes is significantly increased, which can effectively reduce the height of the required cryogenic distillation column, allowing the cryogenic distillation column to be deployed industrially directly in conventional plants (i.e., without the need for deep well technology to install and construct the cryogenic distillation column), thus effectively solving the engineering challenges of implementing isotope cryogenic distillation. At the same time, this application directly uses the chemical exchange method, which is currently industrialized and has a very mature preparation system (compared to cryogenic distillation, it requires significantly less time, and the construction of the required exchange column does not require deep well technology) to assist cryogenic distillation in production, which also has the advantages of being easy to industrialize and requiring a significant reduction in time. Correspondingly, since the entire production process relies on the chemical exchange method and cryogenic distillation to be completed in stages, the entire production process also has the synergistic advantages of the chemical exchange method (short time, low engineering difficulty) and the cryogenic distillation method (simple process, no side reactions, and high product purity).

[0040] It should be noted that, in addition to solving the above-mentioned technical problems and having the above-mentioned advantages, the combined technical solution of this application embodiment can also prepare a full range of products with different abundances according to actual needs. The specific analysis is as follows: (1) It can provide medium abundance (50%~85%). 10 B, this abundance range 10 B is the "golden zone" for many nuclear industry applications and scientific research; (2) it can provide high abundance (≥96%). 10 B, suitable for high-end applications, is a core material for many cutting-edge technologies; (3) can provide ultra-high abundance (≥99%). 10 B, Boron neutron capture therapy (BNCT) is currently the treatment for... 10 The areas with the highest requirements for B abundance, which require... 10 The enrichment level of B needs to exceed 99%.

[0041] It should be noted that before the second stage enrichment of boron isotope intermediates using cryogenic distillation, the boron isotope intermediates obtained in the first stage enrichment can be used directly as the feed gas of the cryogenic distillation column, or the boron isotope intermediates can be subjected to additional abundance homogenization or purification before being used as the feed gas of the cryogenic distillation column.

[0042] It should be noted that this application is the first application of the combination of chemical exchange method and low temperature distillation method in the production of boron isotopes, and the determination of the standard for the combination of the two methods is the core difficulty.

[0043] It should be noted that the enrichment standard for the first stage is strictly controlled to be 40%~90% in the embodiments of this application. This is because if the lower limit of the abundance standard is too low, it is difficult to effectively reduce the height of the cryogenic distillation column (i.e., deep well technology is still required); if the upper limit of the abundance standard is too high, it is equivalent to the entire preparation process becoming dominated by chemical exchange method, which contradicts the starting point of this application, which is that cryogenic distillation method is the core and chemical exchange method is the auxiliary method. This would cause the advantages of cryogenic distillation method, such as simple process, no side reaction and high product purity, to be lost. In addition, it would also introduce problems such as more side reactions, difficult separation and purification, high energy consumption, high equipment requirements and high pollution caused by chemical exchange method enrichment in the high abundance stage.

[0044] As an example, boron isotope intermediates 10 The abundance of B isotopes is 60% to 80%, for example, but not limited to any one of the abundances of 60%, 65%, 70%, 75% and 80% or any range between two.

[0045] In this embodiment, the boron isotope intermediate is... 10 The abundance of B isotopes is limited to the above range, which ensures that the initial feed gas entering the cryogenic distillation column... 10 The lower limit of boron isotope abundance has been further increased, thereby more effectively reducing the required height of cryogenic distillation columns. This allows for easier industrial deployment of cryogenic distillation columns in conventional plants, thus more effectively solving the engineering challenges of implementing isotope cryogenic distillation and correspondingly reducing costs. Simultaneously, the boron isotope intermediates... 10 The abundance upper limit of boron isotopes is limited to the above range. Since the increase in abundance per unit tray of the exchange tower is relatively high within this range, fewer exchange tower stages and a lower single tower height are required during the first stage enrichment using the chemical exchange method. Consequently, the preparation cost required for the first enrichment stage is lower and the preparation efficiency is higher. This allows the overall production cost of boron isotopes to be controlled at a low level while maintaining a high production efficiency, so that both stages can operate stably and efficiently within their respective optimal economic zones.

[0046] It should be noted that the inventors further incorporated boron isotope intermediates into the... 10 The abundance limit of B isotopes is controlled to below 80% because the inventors discovered that the entire preparation process using a single chemical exchange method has the following characteristics: (1) From the perspective of the relationship between separation efficiency and abundance, the chemical exchange method has a higher enrichment efficiency in the low abundance (abundance not exceeding 80%) enrichment stage, and the abundance of each theoretical plate is significantly improved; however, as the product abundance continues to increase, the abundance in the liquid phase decreases. 10As the concentration of B isotopes approaches the equilibrium upper limit, the abundance increase contributed by a unit tray shrinks sharply. The generally accepted mathematical relationship is that the number of theoretical trays N required for separation is logarithmically related to the separation factor α and the abundance ratio at both ends. This means that the proportion of trays required for the high-abundance stage is much higher than the proportion of abundance increase. Specifically, the number of trays required to increase abundance from 80% to 95% is almost twice the number required to increase it from 19.8% to 80%. This implies that the cost of concentrating to the end using a single chemical exchange method is extremely high, and the return on investment drops sharply.

[0047] (2) Although chemical exchange can operate at atmospheric pressure, in high abundance ranges (abundance exceeding 80%), due to the gas-liquid phase in the exchange tower... 10 When the B concentration approaches equilibrium, the reflux ratio must be significantly increased (typically exceeding 200) to continue driving the exchange reaction towards enrichment. However, a high reflux ratio leads to a sharp increase in the gas-liquid load within the column, resulting in a non-linear increase in the required column cross-sectional area and packing volume per unit product, and a dramatic rise in equipment investment and energy consumption. Simultaneously, increasing the reflux ratio also prolongs the production cycle, reduces the yield per unit time, and makes it difficult to achieve higher enrichment levels. Taking the anisole complex method as an example, the entire process of preparation using single chemical exchange distillation typically requires 6–18 exchange columns operating continuously and in coordination, and suffers from the corrosiveness of the complexing agent and some side reactions.

[0048] As an example, in isotopic intermediates 10 The abundance of B isotopes is 65% to 75%, for example, but not limited to any one of the abundance values ​​of 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74% and 75%, or any range between two of them.

[0049] In this embodiment, the boron isotope intermediate is... 10 The abundance of B isotopes is further limited to the aforementioned range, enabling both stages to operate stably and efficiently within their respective optimal economic zones. A detailed analysis follows: (1) The chemical exchange method has the highest abundance contribution increment per unit tray within this abundance range, and the equipment utilization rate and energy consumption ratio are optimal. Specifically, compared with directly exchanging naturally abundant materials through chemical exchange, the chemical exchange method achieves the best results. 10 B isotopes are enriched to an abundance of not less than 96%. In the embodiments of this application, only the naturally abundant isotopes are enriched. 10When boron isotopes are enriched to a level not exceeding 75%, the number of theoretical plates required for chemical exchange towers is only about 30% of that of the former method, and the number of chemical exchange tower stages is reduced from 6-18 stages to 1-3 stages. The difficulty of multi-tower coordination and side reactions are significantly reduced, and the production capacity is increased by at least 80%. At the same time, when using chemical exchange for enrichment in a low-abundance range with a large material throughput, since it does not need to maintain stable operation at -110℃ to -90℃ as in cryogenic distillation, the unit product energy consumption of chemical exchange enrichment can be reduced by 30% to 40% compared to cryogenic distillation in the process of enriching the same amount of material to the same abundance.

[0050] (2) Low-temperature distillation method from an abundance of not less than 65% 10 B isotopes are enriched at high abundance in the target area, compared to directly refining naturally abundant B isotopes through cryogenic distillation. 10 With boron isotope enrichment reaching an abundance of no less than 96%, the theoretical number of trays in the cryogenic distillation section is reduced from thousands to hundreds, and the total height of the column is correspondingly reduced from hundreds of meters to tens of meters. This allows for industrial deployment within conventional plant buildings, completely eliminating the inherent drawbacks of deep underground wells and ultra-high column operation. At the same time, starting from an abundance of 65% and moving towards higher abundances, the purity and process simplicity advantages of cryogenic distillation in the high-abundance section can be fully utilized. Furthermore, since the chemical exchange method does not participate in the enrichment process in the high-abundance section, it can effectively avoid the core drawbacks of the chemical exchange method in the high-abundance section, such as the surge in reflux ratio and the decline in marginal efficiency caused by equilibrium limitations.

[0051] (3) According to the above-mentioned scientific segmented process, the total cost of the combined production process is only 30% to 40% of that of the single chemical exchange process and only 20% to 30% of that of the single low temperature distillation process. This huge economic effect is not a simple series connection of the two preparation processes, but rather a scientific division of labor between the chemical exchange method and the low temperature distillation method in their respective optimal economic zones, so as to generate comprehensive benefits far exceeding those of their independent operation.

[0052] It should be noted that when the isotopic intermediate contains 10 When the abundance of boron isotopes is 65%–75%, the process advantages of both methods are efficiently integrated while effectively avoiding their inherent technical defects. This allows the chemical exchange method and the cryogenic distillation method to be combined in stages, each operating within its optimal economic range. This achieves a synergistic and even multiplicative effect in terms of production efficiency and product cost, rather than a simple addition. This results in a comprehensive improvement of 40%–50% reduction in overall investment, 30%–40% reduction in energy consumption, and an increase in annual production capacity of over 50%. Ultimately, this achieves a comprehensive competitive advantage of "simple process, high purity, low cost, and high yield".

[0053] It should be noted that, since there is no existing technology that combines chemical exchange and cryogenic distillation in stages, and the material state and physicochemical properties during the chemical exchange process after the stages differ significantly from those of the conventional whole-process preparation process, determining the core parameters for each stage is extremely important and extremely difficult.

[0054] As an example, the steps for the first-stage enrichment of naturally abundant BF3 using chemical exchange include: sequentially performing complexation treatment, chemical exchange treatment, pyrolysis separation treatment, and purification treatment on naturally abundant BF3 and an organic complexing agent; wherein, in the chemical exchange treatment step, the total theoretical plate number of the chemical exchange column is 100 to 300 (e.g., but not limited to any one of 100, 150, 200, 250, and 300, or a range between any two), and the reflux ratio is 50 to 200 (e.g., ...). However, not limited to reflux ratios of any one of 50, 80, 100, 120, 140, 160, 180, and 200, or a range between any two; and / or, in the pyrolysis separation step, the pyrolysis separation temperature is 80°C to 220°C (e.g., but not limited to temperatures of any one of 80°C, 100°C, 120°C, 130°C, 140°C, 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, and 220°C, or a range between any two).

[0055] In this embodiment, when the enrichment target for the first stage is 65%~75%, specifically limiting the total theoretical plate number and reflux ratio in the chemical exchange step within the aforementioned range allows for precise matching of the enrichment target, eliminating plate redundancy and reducing unnecessary energy waste. Simultaneously, it ensures the exchange reaction proceeds fully, yielding reaction products with minimal abundance fluctuations and high purity, reducing the difficulty of subsequent separation and purification. Furthermore, when the enrichment target for the first stage is 65%~75%, specifically limiting the pyrolysis separation temperature within the aforementioned range allows for the complete decomposition of the complex between BF3 and the organic complexing agent, leaving no unpyrolyzed complex residue, thereby improving the purity of the product in this stage. This pyrolysis temperature also precisely matches the operating conditions of the upstream chemical exchange column, ensuring a stable output of the 65%~75% target enrichment without significant abundance fluctuations.

[0056] As an example, in the chemical exchange process, the top temperature of the column is 50°C to 100°C (e.g., but not limited to any one of 50°C, 60°C, 70°C, 80°C, 90°C, and 100°C, or a range between any two), the bottom temperature of the column is 60°C to 120°C (e.g., but not limited to any one of 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, and 120°C, or a range between any two), and the reaction pressure is 0.08 MPa to 0.3 MPa (e.g., but not limited to any one of 0.08 MPa, 0.09 MPa, 0.1 MPa, 0.15 MPa, 0.2 MPa, 0.25 MPa, and 0.3 MPa, or a range between any two).

[0057] In this embodiment, when the enrichment target of the first stage is 65%~75% and the total theoretical plate number and reflux ratio of the chemical exchange tower are within a specific range, the top temperature, bottom temperature and reaction pressure of the chemical exchange tower are specifically limited within the above range. This allows the chemical exchange reaction between BF3 and the organic complexing agent to maintain high efficiency and high stability. At the same time, it also allows the temperature, pressure and the total theoretical plate number and reflux ratio to be highly matched, thereby stably and efficiently outputting the reaction product with the target abundance.

[0058] As an example, purification processes include sequentially removing heavy and light substances from materials derived from pyrolysis processes.

[0059] As an example, the first-stage enrichment of naturally abundant BF3 using chemical exchange further includes: cooling the organic complexing agent generated in the pyrolysis and separation step, and then transporting the cooled organic complexing agent to the complexing tower of the complexing step for complexing treatment.

[0060] In this embodiment, the organic complexing agent generated in the pyrolysis and separation step is cooled and then transported to the complexing tower in the complexing treatment step for complexing treatment. This enables a closed-loop process for the organic complexing agent, reduces the amount of fresh organic complexing agent to be replenished, and significantly reduces raw material costs. In particular, cooling the organic complexing agent after high-temperature pyrolysis to a suitable temperature range for the complexing reaction and then reusing it can maintain the temperature stability in the complexing tower, thereby ensuring complexing stability and complexing efficiency.

[0061] It should be noted that during the reuse of the organic complexing agent generated in the pyrolysis and separation step, the organic complexing agent can be directly introduced into the complexing tower, or it can be indirectly introduced into the complexing tower through the feed gas pipeline.

[0062] As an example, the organic complexing agent is selected from at least one of dimethyl ether, diethyl ether, anisole, and methyl isobutyl ketone.

[0063] In this embodiment, a wide variety of organic complexing agents are applicable, providing numerous feasible implementation schemes. This facilitates adaptive adjustments to the type of organic complexing agent used based on the actual production line conditions.

[0064] As an example, the organic complexing agent is selected from anisole.

[0065] In this embodiment, the organic complexing agent is selected from anisole. Anisole can react efficiently with BF3 to form a stable complex, and the separation coefficient of the complex formed by the two is large, which can efficiently separate the boron isotope intermediate with the target abundance. At the same time, anisole also has the advantages of good chemical stability, no strong corrosiveness, low requirements for equipment materials and no need for special anti-corrosion materials.

[0066] It should be noted that since the chemical exchange method is a preparation process that can be industrialized at present and has a very mature preparation system, the processes or steps not specifically described in the embodiments of this application can be carried out in accordance with conventional processes in the field, and this application does not make specific limitations.

[0067] It should be noted that, since there is no existing technology that combines chemical exchange and cryogenic distillation in stages, and the material state and physicochemical properties in the cryogenic distillation process after the stages are quite different from those in the conventional whole-process preparation process, the determination of the core parameters for each stage is extremely important and extremely difficult.

[0068] As an example, in the second-stage enrichment step of boron isotope intermediates using cryogenic distillation, the total theoretical number of plates in the cryogenic distillation column is 400 to 600 (e.g., but not limited to any one of 400, 450, 500, 550, and 600, or any range between two), and the reflux ratio is 50 to 300 (e.g., but not limited to any one of 50, 100, 150, 200, 250, and 300, or any range between two).

[0069] In this embodiment, when the abundance of the feed gas entering the cryogenic distillation column is within the range of 65% to 75%, the total theoretical number of trays and the reflux ratio of the cryogenic distillation column are specifically limited within the above range, which can efficiently and stably generate feed gas with an abundance of not less than 96%. 10 B isotope products; at the same time, the height of the cryogenic distillation column under this process parameter design can be reduced to less than 50 meters, avoiding the inherent defects of high columns being sensitive to wind loads and thermal disturbances. The construction and operation and maintenance costs are reduced by more than 50% compared with the traditional full-process cryogenic distillation process, and the process production cycle under this parameter design can be reduced to 1 to 3 months, which is far lower than the production cycle of several years of the full-process cryogenic distillation process.

[0070] As an example, in a cryogenic distillation column, the top pressure is 0.08 MPa to 0.5 MPa (e.g., but not limited to any one of 0.08 MPa, 0.1 MPa, 0.2 MPa, 0.3 MPa, 0.4 MPa and 0.5 MPa or any range between two), and the top temperature is -110°C to -90°C (e.g., but not limited to any one of -110°C, -105°C, -100°C, -95°C and -90°C or any range between two).

[0071] In this embodiment, when the abundance of the feed gas entering the cryogenic distillation column is 65% to 75% and the total theoretical plate number and reflux ratio of the cryogenic distillation column are both within a specific range, the top pressure and top temperature of the cryogenic distillation column are specifically limited within the above range. This allows the pressure and temperature to be highly matched with the total theoretical plate number and reflux ratio, thereby stably and efficiently generating the target product with an abundance of not less than 96%.

[0072] As an example, the second-stage enrichment of boron isotope intermediates using cryogenic distillation further includes: heating the byproducts generated at the top of the cryogenic distillation column, and then sending the heated byproducts to the chemical exchange column in the chemical exchange treatment step for chemical exchange treatment.

[0073] In this embodiment, the byproducts generated at the top of the cryogenic distillation column ( 10 B (with an abundance typically not less than 50%) is fed into the chemical exchange column after heating for chemical exchange treatment. This enables a closed-loop process for the byproducts generated in the cryogenic distillation column, reducing material waste and thus lowering production costs. Furthermore, reheating and reusing the byproducts generated in the cryogenic distillation column maintains temperature stability within the chemical exchange column, ensuring the stability and efficiency of the chemical exchange treatment. In particular, the byproducts fed back into the chemical exchange column... 10 The abundance of boron is typically no less than 50%, which is much higher than the natural abundance found in chemical exchange towers. 10 B (around 20%) can significantly reduce the separation load in subsequent processes, thereby reducing the overall production energy consumption of the first enrichment stage by more than 30%.

[0074] It should be noted that during the reuse of byproducts generated at the top of the cryogenic distillation column, the byproducts can either enter the cracking column directly or indirectly through the feed gas pipeline.

[0075] In other possible implementations, the byproducts generated at the top of the cryogenic distillation column ( 10B (with an abundance of at least 50%) is fed to a complexation tower in the complexation treatment step after heating to achieve a closed-loop process for the byproducts generated in the low-temperature distillation tower, reduce material waste, and thus lower the preparation cost.

[0076] It should be noted that since low-temperature distillation is a preparation process that can be industrialized at present and has a very mature preparation system, any processes or steps not specifically described in the embodiments of this application can be carried out in accordance with conventional processes in the field, and this application does not make any specific limitations.

[0077] As an example, a process flow diagram of the method for coupling the production of boron isotopes can be found in [reference needed]. Figure 1 .

[0078] To better understand the technical solution, a structural diagram of a production system for coupling the production of boron isotopes is provided here for illustration. For details, please refer to [link / reference needed]. Figure 2 The production system 10 for coupled production of boron isotopes includes a complexing tower 100, a chemical exchange tower 200, a cracking tower 300, a heavy-duty distillation tower 400, a light-duty distillation tower 500, and a cryogenic distillation tower 600 connected sequentially along the material conveying direction. The bottom outlet of the cracking tower 300 (i.e., the outlet of the complexing agent after cracking) is connected to the complexing agent feed pipe of the complexing tower 100, and the lower outlet of the cracking tower 300 (i.e., the outlet of the boron 10 after cracking) is connected to the feed port of the heavy-duty distillation tower 400. The top outlet (i.e., the by-product) of the cryogenic distillation tower 600 is connected to the feed pipe of the boron trifluoride feed gas at the chemical exchange tower 200.

[0079] It should be noted that the specific form of the chemical exchange column 200 and the cryogenic distillation column 600 is not limited. For example, it can be a single column, or a multi-column cascade or multi-column series configuration. The specific form can be adapted to meet actual needs.

[0080] See Figure 3 The chemical exchange tower 200 is a cascaded structure of multiple chemical exchange sub-towers 210, which are designated as 210a, 210b, and so on up to 210n; see reference. Figure 4 The low-temperature distillation column 600 is formed by multiple low-temperature distillation sub-columns 610 connected in series, wherein the multiple low-temperature distillation sub-columns 610 are respectively denoted as 610a, 610b, up to 610n.

[0081] It should be noted that there is no limit to the number of sub-towers that are cascaded or connected in series. The number can be set according to actual needs, such as 2, 3, 4, 5 or 6.

[0082] In this implementation, given a fixed total number of theoretical trays required, cascading or connecting multiple towers in series can effectively reduce the height of a single tower, facilitating industrial deployment within a conventional plant.

[0083] The features and performance of this application will be further described in detail below with reference to the embodiments.

[0084] Example 1 This application provides a method for coupling and producing boron isotopes, employing... Figure 2 The production system shown includes the following steps: The naturally abundant boron trifluoride feedstock gas ( 10 Boron trifluoride (B, with an abundance of 19.8%) and anisole (a complexing agent) were fed into a complexing tower at a molar ratio of 1:1.1 and subjected to complexation treatment at 25°C to generate a boron trifluoride-anisole complex. The material was then fed into a chemical exchange tower for chemical exchange treatment. The chemical exchange tower had a total theoretical plate count of 200, a reflux ratio of 100, a top temperature of 70°C, a bottom temperature of 80°C, and a reaction pressure of 0.15. MPa; then the material is fed into a cracking tower for cracking at 140℃, while the anisole generated in the cracking and separation step is cooled to 25℃, and then the cooled anisole is fed into a complexing tower for complexation; then the material is sequentially fed into a heavy removal distillation tower and a light removal distillation tower for heavy removal and light removal treatment to obtain a boron isotope intermediate with an abundance of 70%; finally, the material is fed into a cryogenic distillation tower for cryogenic distillation, wherein the cryogenic distillation tower has a total theoretical number of 500 plates, a reflux ratio of 150, a top pressure of 0.12 MPa, and a top temperature of -100℃; simultaneously, the by-products generated at the top of the cryogenic distillation tower ( 10 The product (with B abundance ≥ 50%) is heated to 25°C, and then the byproduct after heating is sent to a chemical exchange tower for chemical exchange treatment to obtain a product with an abundance of not less than 96%. 10 Product B.

[0085] Upon testing, the sample prepared in Example 1... 10 Product B has an abundance of 97.2% and a boron trifluoride purity of 99.999%. The cryogenic distillation column has a total height of 48 meters and was installed and operated in a conventional industrial plant without the use of an underground deep well. The production cycle from start-up to steady-state operation of the cryogenic distillation column is 65 days.

[0086] Examples 2-5 are prepared using the same methods as Example 1, except that the total theoretical number of plates, reflux ratio, and pyrolysis temperature of the chemical exchange column, and the total theoretical number of plates and reflux ratio of the cryogenic distillation column are different. For specific parameters and product test results, please refer to Table 1.

[0087] Table 1

[0088] Referring to Table 1, it can be seen that the production of boron isotopes is carried out according to the method provided in the embodiments of this application. 10 Product B has an abundance of over 96% and a boron trifluoride purity of over 99.99%. Furthermore, the total height of the cryogenic distillation tower is as low as 60 meters, allowing it to be installed and operated in a conventional industrial plant without the need for an underground deep well solution.

[0089] Comparative Example 1 This application provides a comparative example of a method for producing boron isotopes, comprising the following steps: The naturally abundant boron trifluoride feedstock gas ( 10 Boron trifluoride (B) with an abundance of 19.8% and anisole (a complexing agent) were fed into a complexing tower at a molar ratio of 1:1.1 and subjected to complexation treatment at 25°C to generate a boron trifluoride-anisole complex. The material was then fed into a chemical exchange tower for chemical exchange treatment. The total theoretical number of plates in the chemical exchange tower was 1000. Figure 3 The process involves a 6-stage cascaded chemical exchange sub-tower configuration, a reflux ratio of 250, a top temperature of 80°C, a bottom temperature of 90°C, and a reaction pressure of 0.15 MPa. The material is then fed into a cracking tower for cracking at 140°C. Simultaneously, the anisole generated in the cracking separation step is cooled to 25°C. The cooled anisole is then fed into a complexing tower for complexation. Finally, the material is sequentially fed into a heavy-weight removal distillation tower and a light-weight removal distillation tower for heavy-weight removal and light-weight removal treatments to obtain a product with an abundance of not less than 96%.

[0090] Comparative Example 2 This application provides a comparative example of a method for producing boron isotopes, comprising the following steps: The naturally abundant boron trifluoride feedstock gas ( 10 (B abundance of 19.8%) is fed into a cryogenic distillation column for cryogenic distillation. The cryogenic distillation column has a total theoretical number of 1200 plates (column height 120 m, requiring underground deep well construction), a reflux ratio of 250, a top pressure of 0.12 MPa, and a top temperature of -100℃; to obtain B with an abundance of not less than 96%. 10 Product B.

[0091] Comparative Example 3 This application provides a comparative example of a method for producing boron isotopes, comprising the following steps: The naturally abundant boron trifluoride feedstock gas ( 10Boron trifluoride (B, with an abundance of 19.8%) and anisole (a complexing agent) were fed into a complexing tower at a molar ratio of 1:1.1 and subjected to complexation treatment at 25°C to generate a boron trifluoride-anisole complex. The material was then fed into a chemical exchange tower for chemical exchange treatment. The chemical exchange tower had a total theoretical plate count of 150, a reflux ratio of 80, a top temperature of 80°C, a bottom temperature of 90°C, and a reaction pressure of 0.15. MPa; then the material is fed to a cracking tower for cracking at 140℃, while the anisole generated in the cracking and separation step is cooled to 40℃, and then the cooled anisole is fed to a complexing tower for complexation; then the material is sequentially fed to a heavy-weight removal distillation tower and a light-weight removal distillation tower for heavy-weight removal and light-weight removal treatment to obtain a boron isotope intermediate with an abundance of 40%; finally, the material is fed to a cryogenic distillation tower for cryogenic distillation, wherein the total theoretical number of trays of the cryogenic distillation tower is 800 (tower height 85 m, requiring underground deep well construction), the reflux ratio is 200, the top pressure is 0.12 MPa, and the top temperature is -100℃; simultaneously, the by-products generated at the top of the cryogenic distillation tower ( 10 The product (with B abundance ≥ 50%) is heated to 25°C, and then the byproduct after heating is sent to a chemical exchange tower for chemical exchange treatment to obtain a product with an abundance of not less than 96%. 10 Product B.

[0092] Comparative Example 4 This application provides a comparative example of a method for producing boron isotopes, comprising the following steps: The naturally abundant boron trifluoride feedstock gas ( 10 Boron trifluoride (B) with an abundance of 19.8% and anisole (a complexing agent) were fed into a complexing tower at a molar ratio of 1:1.1 and subjected to complexation treatment at 25°C to generate a boron trifluoride-anisole complex. The material was then fed into a chemical exchange tower for chemical exchange treatment. The total theoretical number of plates in the chemical exchange tower was 700. Figure 3The process involves a 4-stage cascade of chemical exchange sub-towers, a reflux ratio of 220, a top temperature of 85°C, a bottom temperature of 90°C, and a reaction pressure of 0.15 MPa. The material is then fed into a cracking tower for cracking at 140°C. Simultaneously, the anisole generated in the cracking separation step is cooled to 40°C, and then fed into a complexing tower for complexation. The material is then sequentially fed into a heavy-weight removal distillation tower and a light-weight removal distillation tower for heavy-weight removal and light-weight removal treatment to obtain a boron isotope intermediate with an abundance of 90%. Finally, the material is fed into a cryogenic distillation tower for cryogenic distillation. The cryogenic distillation tower has a total theoretical number of 350 plates (tower height 35 m, no need for underground deep well construction), a reflux ratio of 100, a top pressure of 0.12 MPa, and a top temperature of -100°C. Simultaneously, the byproducts generated at the top of the cryogenic distillation tower are processed. 10 The product (with B abundance ≥ 50%) is heated to 25°C, and then the byproduct after heating is sent to a chemical exchange tower for chemical exchange treatment to obtain a product with an abundance of not less than 96%. 10 Product B.

[0093] To better understand the differences between Example 1 and the various comparative examples, a summary is provided here in tabular form, as detailed in Table 2.

[0094] Table 2

[0095] Referring to Table 2, the test results of Example 1 and Comparative Examples 1-2 show that the method for coupled production of boron isotopes provided in the embodiments of this application can effectively solve the engineering problems existing in implementing the low-temperature distillation method of isotopes compared with the single chemical exchange method or the single low-temperature distillation method. It also has the synergistic advantages of the chemical exchange method (short time, low engineering difficulty) and the low-temperature distillation method (simple process, no side reactions, and high product purity).

[0096] As can be seen from the test results of Example 1 and Comparative Examples 3-4, controlling the switching point within a suitable range can effectively solve the engineering problems existing in implementing the isotope cryogenic distillation method compared to the switching point not being within a suitable range. It also has the advantages of short production cycle and low production cost.

[0097] The embodiments described above are some, but not all, of the embodiments of this application. The detailed description of the embodiments of this application is not intended to limit the scope of the claimed application, but merely to illustrate selected embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

Claims

1. A method for coupling the production of boron isotopes, characterized in that, Includes the following steps: The first-stage enrichment of naturally abundant BF3 was performed using a chemical exchange method to obtain boron isotope intermediates. 10 The abundance of B isotopes is 50%–85%; The boron isotope intermediate was enriched in a second stage using a low-temperature distillation method until... 10 The abundance of B isotopes is not less than 96%.

2. The method for coupling and producing boron isotopes according to claim 1, characterized in that, The boron isotope intermediate 10 The abundance of B isotopes is 60%–80%.

3. The method for coupling and producing boron isotopes according to claim 2, characterized in that, The boron isotope intermediate 10 The abundance of B isotopes is 65%–75%.

4. The method for coupling production of boron isotopes according to claim 3, characterized in that, The first-stage enrichment of naturally abundant BF3 using chemical exchange includes: Naturally abundant BF3 and organic complexing agents were subjected to complexation treatment, chemical exchange treatment, cleavage separation treatment and purification treatment in sequence; In the chemical exchange treatment step, the total number of theoretical plates in the chemical exchange tower is 100 to 300, and the reflux ratio is 50 to 200; and / or, in the pyrolysis separation treatment step, the pyrolysis separation temperature is 80℃ to 220℃.

5. The method for coupling and producing boron isotopes according to claim 4, characterized in that, In the chemical exchange treatment step, the top temperature of the column is 50℃~100℃, the bottom temperature of the column is 60℃~120℃, and the reaction pressure is 0.08 MPa~0.3 MPa.

6. The method for coupling production of boron isotopes according to claim 4, characterized in that, The first-stage enrichment step of naturally abundant BF3 using chemical exchange method also includes: The organic complexing agent generated in the pyrolysis and separation process is cooled down, and then the cooled organic complexing agent is transported to the complexing tower of the complexing process for complexing treatment.

7. The method for coupling and producing boron isotopes according to claim 4, characterized in that, The organic complexing agent is selected from at least one of dimethyl ether, diethyl ether, anisole, and methyl isobutyl ketone; Optionally, the organic complexing agent is selected from anisole.

8. The method for coupling production of boron isotopes according to claim 3, characterized in that, In the step of enriching the boron isotope intermediate in the second stage using a low-temperature distillation method, the total theoretical number of plates in the low-temperature distillation column is 400 to 600, and the reflux ratio is 50 to 300.

9. The method for coupling production of boron isotopes according to claim 8, characterized in that, In the aforementioned cryogenic distillation column, the top pressure is 0.08 MPa to 0.5 MPa and the top temperature is -110℃ to -90℃.

10. The method for coupling production of boron isotopes according to claim 4, characterized in that, The step of enriching the boron isotope intermediate in a second stage using low-temperature distillation further includes: The byproducts generated at the top of the low-temperature distillation column are heated, and then the heated byproducts are transported to the chemical exchange column in the chemical exchange treatment step for chemical exchange treatment.

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