A method for separation and enrichment of boron-10 isotope

Abstract

The invention provides a boron-10 isotope separation and enrichment method. The boron-10 isotope separation and enrichment method comprises at least two stages of separation and enrichment reaction units, and each stage of the separation and enrichment reaction unit comprises a complex reaction, an exchange reaction and a desorption reaction, which can fully ensure that each stage of the separation and enrichment reaction unit promotes the chemical equilibrium in a positive direction, so that the boron-10 isotope is enriched in a liquid phase until the boron-10 isotope abundance reaches more than 96%, and according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained; the boron-10 isotope separation and enrichment method of the invention has not only a simple process and low equipment requirements, but also can greatly reduce the height of an exchange tower, and can also provide boron-10 isotope products with different abundances.

Description

[0001] This invention is a divisional application of the invention patent application with Chinese national application number 202411322000.3, application date September 23, 2024, and invention name “A boron-10 isotope separation and enrichment device and separation and enrichment method”. Technical Field

[0002] The invention relates to the technical field of boron-10 isotope separation, and in particular to a boron-10 isotope separation and enrichment method. Background Art

[0003] Stable isotope boron-10 ( 10 B) Due to its unique neutron absorption characteristics, it is increasingly used in modern nuclear industry, military equipment and medicine. 10 B products include boron-10 acid, boron-10 powder, boron carbide, boron nitride and other products with different abundance requirements. The industrial chain is long and the product application fields are wide, especially playing an important role in alleviating the global petrochemical energy shortage. The application of such products in the nuclear energy field makes it possible to widely develop and apply economic, safe and clean nuclear energy resources.

[0004] Since the isotope boron-10 has a much larger thermal neutron capture area than boron-11, it is widely used in the nuclear industry to manufacture thermal neutron counters, reactor control rods and thermal neutron shielding materials, especially in boron neutron cancer treatment methods (BNCT). The abundance of boron-10 in nature is only 19-20%, so it is necessary to enrich and purify the boron-10 isotope.

[0005] The chemical exchange distillation method of boron trifluoride anisole is a process technology first invented in the United States. It started in the mid-1970s and reached full production in 1977 with a production scale of 2 tons / year, and the boron-10 abundance can reach 92%. This process technology has advantages because it operates under normal temperature and pressure conditions and has a higher separation coefficient. Although the process of preparing anisole complex from raw materials is slightly longer than that of methyl and ethyl ether complex materials, its basic material anisole is recycled in the whole process of the production system, and the final product is enriched boron trifluoride-10 ( 10 BF 3 ) and boron trifluoride-11( 11 BF 3 ), both of which are high value-added terminal technology products, in terms of cost and benefit accounting, compared with the methyl ether method, ethyl ether method has obvious advantages, making the production cost much lower. Currently, the United States and Georgia both use this process technology route.

[0006] However, due to the long process, many sub-processes and complex operations, industrial production is difficult. 10B separation requires a chemical exchange tower with many theoretical plates and a tower height of over 100 meters, which places high demands on equipment and makes industrialization difficult.

[0007] CN102773016A discloses a method and device for separating and enriching boron-10 by connecting multiple towers in series, which realizes the separation by connecting multiple chemical exchange towers in series. 10 B enrichment production; the production device mainly includes a complexing tower, a chemical exchange tower in series, and a cracking tower; a condenser is provided at the top of the cracking tower, and a heating kettle is provided at the bottom of the tower; a pump is used to realize the continuous flow of the liquid phase between the complexing tower, each chemical exchange tower and the cracking tower. The liquid phase sprayed down from the complexing tower is pumped to the top of the first chemical exchange tower, and then pumped to the top of the second chemical exchange tower after flowing out from the bottom of the tower, until the liquid phase coming out from the bottom of the last exchange tower is pumped to the top of the cracking tower, and the liquid phase flowing out from the bottom of the cracking tower is heat exchanged through a heat exchanger, and then pumped to the top of the complexing tower, thereby forming a circulating flow of the liquid phase between the series towers. However, this technical solution cannot obtain boron-10 isotope products of different abundances.

[0008] In summary, there is a need to develop a method for separation and enrichment of boron-10 isotopes, which is not only simple in process and has low equipment requirements, but can also provide boron-10 isotope products with different abundances. Summary of the invention

[0009] In view of the problems existing in the prior art, the present invention provides a boron-10 isotope separation and enrichment device and a separation and enrichment method. The boron-10 isotope separation and enrichment device comprises at least two groups of separation and enrichment units connected in series, and each group of the separation and enrichment units comprises a complexing tower, an exchange tower, and a desorption tower connected in sequence, which can fully ensure that each group of separation and enrichment units can promote the chemical equilibrium in a positive direction, so that the boron-10 isotope is enriched in the liquid phase until the boron-10 isotope abundance reaches more than 96%, and according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained; the boron-10 isotope separation and enrichment device of the present invention not only has a simple process and low equipment requirements, but also can greatly reduce the height of the exchange tower, and can also provide boron-10 isotope products with different abundances.

[0010] To achieve this object, the present invention adopts the following technical solutions:

[0011] One of the purposes of the present invention is to provide a boron-10 isotope separation and enrichment device, the boron-10 isotope separation and enrichment device comprising at least two groups of separation and enrichment units connected in series;

[0012] Each group of separation and enrichment units comprises a complexing tower, an exchange tower, and a desorption tower connected in sequence; the complexing tower is provided with a complexing agent inlet, an uncomplexed boron trifluoride gas outlet, a complex product outlet, and a complex reaction boron trifluoride gas inlet; the exchange tower is provided with a complex inlet, an exchanged boron trifluoride gas outlet, an exchange reaction boron trifluoride gas inlet, and an exchange product outlet; the desorption tower is provided with a liquid inlet, a desorbed gas outlet, and a desorbed liquid outlet; the complex product outlet is connected to the complex inlet, the complex reaction boron trifluoride gas inlet is connected to the exchanged boron trifluoride gas outlet, and the exchange product outlet is connected to the liquid inlet;

[0013] The desorbed gas outlet in the upper group of separation and enrichment units is connected to the exchange reaction boron trifluoride gas inlet in the lower group of separation and enrichment units; the uncomplexed boron trifluoride gas outlet in the lower group of separation and enrichment units is connected to the complex reaction boron trifluoride gas inlet in the upper group of separation and enrichment units;

[0014] The exchange reaction boron trifluoride gas inlet of the exchange tower in the first group of separation and enrichment units is connected to the boron trifluoride gas raw material, which is used to provide the boron trifluoride gas raw material; the uncomplexed boron trifluoride gas outlet of the complex tower in the first group of separation and enrichment units is used to collect boron trifluoride-11 gas;

[0015] The complexing agent inlet of the complexing tower in each group of the separation and enrichment units is used to provide the complexing agent, and the desorbed liquid outlet of the desorption tower in each group of the separation and enrichment units is used to recover and purify the complexing agent.

[0016] The chemical exchange distillation method of boron trifluoride anisole mainly includes three reactions, namely the complexation reaction of boron trifluoride and anisole, the reaction of boron trifluoride-10( 10 BF 3 ) and anisole-boron trifluoride-11( 11 BF 3 ) complex exchange reaction, desorption reaction of anisole-boron trifluoride complex; the complex reaction between boron trifluoride and anisole complexing agent is an exothermic reversible reaction, and the exchange coefficient of the exchange reaction is very small, about 1.03. To achieve a good separation and purification rate, a longer exchange time is usually required, that is, the exchange tower needs a larger height, generally 20 meters, or even more than 40 meters, and different process conditions are required to obtain products with different boron-10 isotope abundances.

[0017] In this regard, the prior art discloses a method of connecting multiple chemical exchange towers in series to achieve 10The technical solution for the enrichment production of B is a method of connecting multiple exchange towers in series. The liquid phase sprayed down from the complexing tower is pumped to the top of the first chemical exchange tower, flows out from the bottom of the tower and is then pumped to the top of the second chemical exchange tower, until the liquid phase coming out from the bottom of the last exchange tower is pumped to the top of the cracking tower, the liquid phase flowing out from the bottom of the cracking tower is heat exchanged through a heat exchanger, and is then pumped to the top of the complexing tower, thereby forming a circulating flow of the liquid phase between the series-connected towers, and the gas phase at the top of the cracking tower enters the bottom of the last exchange tower, flows out from the top of the tower and enters the bottom of the previous chemical exchange tower, until the liquid phase coming out from the top of the first exchange tower enters the bottom of the complexing tower and is collected from the top of the complexing tower, thereby forming a circulating flow of the gas phase between the series-connected towers.

[0018] The inventors have found that simply connecting multiple exchange towers in series, that is, simply carrying out multi-stage series exchange reactions, whether it is liquid or gas phase materials, requires repeated changes in the height of the top and bottom of the tower during the circulation process, resulting in unstable temperature and pressure states of the reaction system, which limits the effect of promoting the chemical equilibrium of the exchange reaction, and there is still great room for improvement. In this regard, the boron-10 isotope separation and enrichment device of the present invention includes at least two groups of separation and enrichment units connected in series, and each group of the separation and enrichment units includes a complexing tower, an exchange tower, and a desorption tower connected in sequence, so that the higher abundance boron-10 isotope obtained by each group of separation and enrichment units can enter the next group of separation and enrichment units in the form of boron trifluoride gas, and the complexing reaction, exchange reaction and desorption reaction of each group of separation and enrichment units can ensure the effect of promoting chemical equilibrium. Therefore, based on the positive advancement of the chemical equilibrium by each group of separation and enrichment units, the boron-10 isotope is enriched in the liquid phase until the boron-10 isotope abundance reaches more than 96%. Moreover, according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained.

[0019] The operation process of the boron-10 isotope separation and enrichment device of the present invention includes: boron trifluoride gas is adsorbed by anisole in a complexing tower to form a complex, and the unabsorbed boron trifluoride is collected and purified and then enters the complexing tower of the previous group of separation devices. The complexed anisole-boron trifluoride liquid enters the exchange tower from the top and exchanges with the boron trifluoride entering from the bottom as shown below:

[0020] C 6 H 5 OCH 3 g 11 BF 3(l) + 10 BF 3(g) →C 6 H 5 OCH 3 g 10 BF 3(l) +11 BF 3(g)

[0021] The exchanged boron trifluoride gas enters the complexation tower from the top, and the exchanged anisole-boron trifluoride liquid enters the desorption tower from the bottom. The anisole-boron trifluoride liquid in the desorption tower is heated and decomposed into anisole, boron trifluoride gas and anisole. After purification and drying, the anisole enters the raw material tank for recycling in the complexation tower, and the boron trifluoride gas enters the next group of exchange towers according to the abundance requirements to further increase the abundance of boron-10 or enters the hydrolysis tower to obtain a product with a specified abundance. In the exchange tower, gaseous boron trifluoride-10 is continuously exchanged with liquid anisole-boron trifluoride-11 to generate anisole-boron trifluoride-10 and gaseous boron trifluoride-11, that is, the boron-11 isotope is enriched in the gaseous state and the boron-10 isotope is enriched in the liquid state, thereby achieving the purpose of boron isotope separation and purification.

[0022] The invention adopts a multi-stage exchange structure, which can greatly reduce the height of the exchange tower, and can obtain a variety of products with different boron-10 isotope abundances as needed. In addition, in the boron trifluoride anisole exchange separation process, the separation temperature has a greater impact on the separation effect. After the height of the exchange tower is reduced, the whole set of devices can be placed indoors, thereby reducing the energy consumption in the constant temperature process of the exchange tower and improving the temperature stability.

[0023] As a preferred technical solution of the present invention, the boron-10 isotope separation and enrichment device also includes a complexing agent purification and drying device; the complexing agent inlet of the complexing tower in each group of the separation and enrichment units is connected to the outlet of the complexing agent purification and drying device, so as to provide complexing agent for the complexing tower in each group of the separation and enrichment units; the desorbed liquid outlet of the desorption tower in each group of the separation and enrichment units is connected to the inlet of the complexing agent purification and drying device, so as to purify and dry the recovered complexing agent obtained by the desorption tower in each group of the separation and enrichment units for recycling.

[0024] As a preferred technical solution of the present invention, the complexing agent purification and drying device comprises a distillation tower and a drying tower connected in series in sequence, that is, the complexing agent purification and drying device of the present invention first purifies the complexing agent by a distillation method through a distillation tower, and then the purified complexing agent enters the drying tower for drying to avoid the influence of water impurities on separation and purification; wherein, those skilled in the art can select distillation towers of different specifications according to the amount of complexing agent used.

[0025] As a preferred technical solution of the present invention, the height of the distillation tower is 3-5m, for example, 3m, 3.5m, 4m, 4.5m or 5m.

[0026] As a preferred technical solution of the present invention, the height of the drying tower is 1-2m, for example, 1m, 1.1m, 1.3m, 1.5m, 1.7m, 1.8m or 2m.

[0027] As a preferred technical solution of the present invention, the drying tower is filled with molecular sieves.

[0028] It should be noted that the complexing agent purification and drying device of the present invention also includes a complexing agent storage tank arranged at the outlet of the purification tower, and those skilled in the art can also perform secondary drying in the drying tower before the complexing agent enters the separation and enrichment device according to actual needs.

[0029] As a preferred technical solution of the present invention, the exchange towers in each group of the separation and enrichment units have a tower height of 5-10 m, such as 5 m, 6 m, 7 m, 8 m, 9 m or 10 m.

[0030] As a preferred technical solution of the present invention, a purification tower is set at the inlet of the boron trifluoride gas of the exchange reaction of the exchange tower in the first group of separation and enrichment units, so that the boron trifluoride gas raw material is purified before separation and enrichment; the purification tower is filled with fluoride salt for adsorbing free hydrogen fluoride in the boron trifluoride gas raw material.

[0031] The present invention also provides a boron-10 isotope separation and enrichment method, which comprises at least two stages of separation and enrichment reaction units, each stage of which comprises a complexation reaction, an exchange reaction and a desorption reaction:

[0032] The boron trifluoride gas raw material undergoes a first-stage exchange reaction with the complex product from the first-stage complex reaction; after the exchange, the boron trifluoride gas undergoes a first-stage complex reaction with the complexing agent to generate a complex product; the exchange product after the exchange undergoes a first-stage desorption reaction; the gas after desorption enters the next-stage exchange reaction to enrich a higher-abundance boron-10 isotope in the liquid phase, or, according to the boron-10 isotope abundance requirement, a portion of the gas after desorption is taken out and hydrolyzed to obtain boric acid for collection;

[0033] The desorbed gas obtained from the previous desorption reaction undergoes an exchange reaction at this stage with the complex product obtained from the current complex reaction; the boron trifluoride gas after the exchange undergoes a complex reaction at this stage with the complexing agent to generate a complex product, and the uncomplexed boron trifluoride gas enters the previous complex reaction to ensure sufficient complexation; the exchange product after the exchange undergoes a desorption reaction at this stage; the desorbed gas enters the next exchange reaction to enrich a higher abundance boron-10 isotope in the liquid phase, or, according to the boron-10 isotope abundance requirement, part of the desorbed gas is taken out and the boric acid is obtained by hydrolysis and collected;

[0034] Based on the positive advancement of chemical equilibrium by the complexation reaction, exchange reaction and desorption reaction at each stage, the boron-10 isotope is enriched in the liquid phase until the boron-10 isotope abundance reaches more than 96%. In addition, according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained, and the first-stage complexation reaction collects the boron-11 isotope by-product.

[0035] It should be noted that the boron-10 isotope separation and enrichment method described in the present invention is preferably carried out using the aforementioned boron-10 isotope separation and enrichment device, that is, at least two stages of separation and enrichment reaction units correspond to at least two groups of separation and enrichment units connected in series, and the complexation reaction, exchange reaction and desorption reaction of each stage of the separation and enrichment reaction unit are respectively carried out in the complexation tower, exchange tower and desorption tower connected in sequence to each group of the separation and enrichment units.

[0036] The boron-10 isotope separation and enrichment method of the present invention comprises at least two stages of separation and enrichment reaction units, and each stage of the separation and enrichment reaction unit comprises a complexation reaction, an exchange reaction and a desorption reaction, which can fully ensure that each stage of the separation and enrichment reaction unit promotes the chemical equilibrium in a positive direction, so that the boron-10 isotope is enriched in the liquid phase until the boron-10 isotope abundance reaches more than 96%, and according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained; the boron-10 isotope separation and enrichment method of the present invention not only has a simple process and low equipment requirements, but also can greatly reduce the height of the exchange tower, and can also provide boron-10 isotope products with different abundances.

[0037] As a preferred technical solution of the present invention, in each group of separation and enrichment units, the temperature of the complexing tower is independently 10-35°C, for example, 10°C, 13°C, 15°C, 17°C, 20°C, 23°C, 25°C, 28°C, 30°C, 31°C, 33°C or 35°C, etc.

[0038] As a preferred technical solution of the present invention, in each group of separation and enrichment units, the reflux ratio of the exchange tower is independently (200-250):1, for example, 200:1, 210:1, 220:1, 230:1, 240:1 or 250:1, etc.

[0039] As a preferred technical solution of the present invention, in each group of separation and enrichment units, the temperature of the exchange tower is independently 20-30°C, for example, 20°C, 21°C, 23°C, 25°C, 26°C, 28°C or 30°C.

[0040] As a preferred technical solution of the present invention, in each group of separation and enrichment units, the temperature of the desorption tower is independently 140-160°C, such as 140°C, 145°C, 150°C, 155°C or 160°C.

[0041] As a preferred technical solution of the present invention, the desorbed liquid from the desorption tower in each group of separation and enrichment units enters the complexing agent purification and drying device for purification and drying, and the recovered complexing agent enters the complexing tower in each group of separation and enrichment units for complexing reaction.

[0042] Compared with the prior art solutions, the present invention has at least the following beneficial effects:

[0043] The invention provides a boron-10 isotope separation and enrichment device. The boron-10 isotope separation and enrichment device comprises at least two groups of separation and enrichment units connected in series, and each group of the separation and enrichment units comprises a complexing tower, an exchange tower, and a desorption tower connected in sequence, which can fully ensure that each group of separation and enrichment units can promote the chemical equilibrium in a positive direction, so that the boron-10 isotope is enriched in a liquid phase until the boron-10 isotope abundance reaches more than 96%. Moreover, according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained. The boron-10 isotope separation and enrichment device of the invention has not only a simple process and low equipment requirements, but also can greatly reduce the height of the exchange tower and can provide boron-10 isotope products with different abundances. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 is a schematic diagram of the boron-10 isotope separation and enrichment device described in Example 1 of the present invention;

[0045] In the figure: 1-complexation tower; 2-exchange tower; 3-desorption tower; 4-complexation agent purification and drying device. DETAILED DESCRIPTION

[0046] The technical solution of the present invention is further described below with reference to the accompanying drawings and through specific implementation methods.

[0047] To better illustrate the present invention and facilitate understanding of the technical solution of the present invention, typical but non-limiting embodiments of the present invention are as follows:

[0048] Example 1

[0049] This embodiment provides a boron-10 isotope separation and enrichment device, such as Figure 1 As shown, the boron-10 isotope separation and enrichment device includes three groups of separation and enrichment units connected in series;

[0050] like Figure 1As shown, each group of separation and enrichment units connected in series is framed by dotted lines, and each group of separation and enrichment units includes a complexing tower 1, an exchange tower 2, and a desorption tower 3 connected in sequence; the complexing tower 1 is provided with a complexing agent inlet, an uncomplexed boron trifluoride gas outlet, a complex product outlet, and a complex reaction boron trifluoride gas inlet; the exchange tower 2 is provided with a complex inlet, an exchanged boron trifluoride gas outlet, an exchange reaction boron trifluoride gas inlet, and an exchange product outlet; the desorption tower 3 is provided with a liquid inlet, a desorbed gas outlet, and a desorbed liquid outlet; the complex product outlet is connected to the complex inlet, the complex reaction boron trifluoride gas inlet is connected to the exchanged boron trifluoride gas outlet, and the exchange product outlet is connected to the liquid inlet;

[0051] The desorbed gas outlet in the upper group of separation and enrichment units is connected to the exchange reaction boron trifluoride gas inlet in the lower group of separation and enrichment units; the uncomplexed boron trifluoride gas outlet in the lower group of separation and enrichment units is connected to the complex reaction boron trifluoride gas inlet in the upper group of separation and enrichment units;

[0052] The boron-10 isotope separation and enrichment device also includes a complexing agent purification and drying device 4; the complexing agent purification and drying device includes a distillation tower and a drying tower connected in series in sequence; the complexing agent inlet of the complexing tower 1 in each group of the separation and enrichment units is connected to the outlet of the drying tower of the complexing agent purification and drying device 4, so as to provide complexing agent for the complexing tower 1 in each group of the separation and enrichment units; the desorbed liquid outlet of the desorption tower 3 in each group of the separation and enrichment units is connected to the inlet of the distillation tower of the complexing agent purification and drying device 4, so as to purify and dry the recovered complexing agent obtained by the desorption tower 3 in each group of the separation and enrichment units for recycling;

[0053] In the complexing agent purification and drying device 4, the distillation tower has a height of 4m; the drying tower has a height of 1.5m; the drying tower is filled with molecular sieves; the exchange tower in each group of the separation and enrichment units has a height of 6m;

[0054] The exchange reaction boron trifluoride gas inlet of the exchange tower 2 in the first group of separation and enrichment units is used to provide BF 3 The first group of separation and enrichment units in the complex tower 1 of the uncomplexed boron trifluoride gas outlet for collecting 11 BF 3 The third group of separation and enrichment unit desorption tower 3 after desorption gas outlet for collecting 10 BF 3 The desorbed gas outlet of the desorber 3 in the other separation and enrichment units is also provided with a branch pipeline, which can collect different abundances as needed. 10 BF 3 product;

[0055] based on Figure 1 The present embodiment also provides a boron-10 isotope separation and enrichment method, wherein anisole is selected as the complexing agent, and the boron-10 isotope separation and enrichment method comprises the following contents:

[0056] BF 3 The raw material enters the exchange tower 2 in the first group of separation and enrichment units, and undergoes an exchange reaction with the complex product from the complex tower 1 in the first group of separation and enrichment units; the boron trifluoride gas after the exchange enters the complex tower 1 in the first group of separation and enrichment units, and undergoes a complex reaction with the complexing agent to generate a complex product; the exchange product after the exchange enters the desorption tower 3 in the first group of separation and enrichment units for a desorption reaction; the desorbed gas enters the exchange tower 2 in the next group of separation and enrichment units for enrichment of a higher abundance boron-10 isotope in the liquid phase, or, according to the boron-10 isotope abundance requirement, a portion of the desorbed gas is taken out, and the boric acid is obtained by hydrolysis for collection;

[0057] In the next group of separation and enrichment units, the desorbed gas from the previous group undergoes an exchange reaction at this stage with the complex product of the complex tower 1 of this group; the exchanged boron trifluoride gas enters the complex tower 1 of this group, undergoes a complex reaction at this stage with the complexing agent to generate a complex product, and the uncomplexed boron trifluoride gas enters the complex tower 1 in the previous group of separation and enrichment units to ensure sufficient complexation; the exchanged exchange product enters the desorption tower 3 of this group to undergo a desorption reaction at this stage; the desorbed gas enters the exchange tower 2 in the next group of separation and enrichment units to enrich a higher abundance boron-10 isotope in the liquid phase, or, according to the boron-10 isotope abundance requirement, a portion of the desorbed gas is taken out and hydrolyzed to obtain boric acid for collection;

[0058] Based on the positive advancement of the chemical equilibrium by each group of separation and enrichment units, that is, based on the positive advancement of the chemical equilibrium by the complexation reaction, exchange reaction and desorption reaction at each stage, the boron-10 isotope is enriched in the liquid phase; the uncomplexed boron trifluoride gas outlet of the complexation tower 1 in the first group of separation and enrichment units is used to collect 11 BF 3 The third group of separation and enrichment unit desorption tower 3 after desorption gas outlet for collecting 10 BF 3 The desorbed gas outlet of the desorber 3 in the other separation and enrichment units is also provided with a branch pipeline, which can collect different abundances as needed. 10 BF 3 product;

[0059] wherein, boron trifluoride gas is purified and dehydrofluorinated before entering the reactor, anisole is purified to remove impurities such as phenol produced by decomposition, and then dried to a water exchange amount of less than 100 ppm before participating in the exchange; in each group of separation and enrichment units, the temperature of the complexing tower is independently 20°C; in each group of separation and enrichment units, the temperature of the exchange tower is independently 25°C, and the reflux ratio of the exchange tower is set to 210:1; in each group of separation and enrichment units, the temperature of the desorption tower is independently 150°C; the desorbed liquid of the desorption tower in each group of separation and enrichment units enters the complexing agent purification and drying device for purification and drying, and the recovered complexing agent enters the complexing tower in each group of separation and enrichment units for complexing reaction;

[0060] The desorption tower in the first set of separation and enrichment units can obtain 60% of the abundance 10 BF 3 The product gas is hydrolyzed to obtain boric acid; the desorption tower in the second set of separation and enrichment units can obtain 80% of the abundance 10 BF 3 The product gas is hydrolyzed to obtain boric acid; the desorption tower in the third group of separation and enrichment units can obtain an abundance of more than 96%. 10 BF 3 The product gas is hydrolyzed to obtain boric acid.

[0061] Comparative Example 1

[0062] This comparative example provides a boron-10 isotope separation and enrichment device, which is based on CN102773016A Figure 1 The device shown has three exchange towers connected in series, a complexing tower at the raw material inlet, and a desorption tower at the product outlet.

[0063] This comparative example also provides a method for separating and enriching boron-10 isotopes, which is carried out using the device described in the comparative example above, with the temperature of the complexing tower being 20°C; the temperature of each group of exchange towers being independently 25°C, and the reflux ratio of the exchange towers being set to 210:1; and the temperature of the desorption towers being independently 150°C. The abundance of 65% is obtained at the bottom of the last exchange tower. 10 BF 3 Product gas.

[0064] In summary, the present invention provides a boron-10 isotope separation and enrichment device and a separation and enrichment method. The boron-10 isotope separation and enrichment device comprises at least two groups of separation and enrichment units connected in series, and each group of the separation and enrichment units comprises a complexing tower, an exchange tower, and a desorption tower connected in sequence, which can fully ensure that each group of separation and enrichment units promotes the chemical equilibrium in a positive direction, so that the boron-10 isotope is enriched in the liquid phase until the boron-10 isotope abundance reaches more than 96%, and according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained; the boron-10 isotope separation and enrichment device of the present invention not only has a simple process and low equipment requirements, but also can greatly reduce the height of the exchange tower, and can also provide boron-10 isotope products with different abundances.

[0065] The present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the components selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0066] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0067] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0068] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A method for separation and enrichment of boron-10 isotopes, characterized in that: The boron-10 isotope separation and enrichment method comprises at least two stages of separation and enrichment reaction units, each stage of the separation and enrichment reaction unit comprises a complexation reaction, an exchange reaction and a desorption reaction: The boron trifluoride gas raw material undergoes a first-stage exchange reaction with the complex product from the first-stage complex reaction; after the exchange, the boron trifluoride gas undergoes a first-stage complex reaction with the complexing agent to generate a complex product; the exchange product after the exchange undergoes a first-stage desorption reaction; the gas after desorption enters the next-stage exchange reaction to enrich a higher-abundance boron-10 isotope in the liquid phase, or, according to the boron-10 isotope abundance requirement, a portion of the gas after desorption is taken out and hydrolyzed to obtain boric acid for collection; The desorbed gas obtained from the previous desorption reaction undergoes an exchange reaction at this stage with the complex product obtained from the current complex reaction; the boron trifluoride gas after the exchange undergoes a complex reaction at this stage with the complexing agent to generate a complex product, and the uncomplexed boron trifluoride gas enters the previous complex reaction to ensure sufficient complexation; the exchange product after the exchange undergoes a desorption reaction at this stage; the desorbed gas enters the next exchange reaction to enrich a higher abundance boron-10 isotope in the liquid phase, or, according to the boron-10 isotope abundance requirement, part of the desorbed gas is taken out and the boric acid is obtained by hydrolysis and collected; Based on the positive advancement of chemical equilibrium by the complexation reaction, exchange reaction and desorption reaction at each stage, the boron-10 isotope is enriched in the liquid phase until the boron-10 isotope abundance reaches more than 96%. In addition, according to different boron-10 isotope abundance requirements, boron-10 isotope products with different abundances can be obtained, and the first-stage complexation reaction collects the boron-11 isotope by-product.

2. The boron-10 isotope separation and enrichment method according to claim 1, characterized in that: The temperature of each stage of complexation reaction is independently 10-35°C.

3. The boron-10 isotope separation and enrichment method according to claim 1, characterized in that: The reflux ratio of each exchange reaction is independently (200-250):

1.

4. The boron-10 isotope separation and enrichment method according to claim 1, characterized in that: The temperature of each exchange reaction is independently 20-30°C.

5. The boron-10 isotope separation and enrichment method according to claim 1, characterized in that: The temperature of each stage of desorption reaction is independently 140-160°C.

6. The boron-10 isotope separation and enrichment method according to any one of claims 1 to 5, characterized in that: The desorbed liquid of each stage of desorption reaction is purified and dried, and the recovered complexing agent is respectively introduced into each stage of complexing reaction for use in the complexing reaction.

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