Process and apparatus for high-quality separation of boron isotopes

Abstract

The application provides a process and device for high-quality boron isotope separation, comprising an exchange rectification system, a complexing system, a complex cracking system and a boron-11 refining system, natural abundance boron trifluoride isotopes are separated through the exchange rectification tower, and the circulation and regeneration of boron trifluoride and anisole are realized through the complexing system and the cracking system. The boron-11 refining system is arranged to further improve the abundance of boron-11. The application can realize the industrialized continuous production of 99% abundance high-quality boron-10 trifluoride and 99.9% abundance high-quality boron-11 trifluoride simultaneously, and the process is simple and has strong operability.

Description

Technical Field

[0001] This invention belongs to the field of boron isotope separation and production, specifically relating to a process and apparatus for separating and producing high-quality boron-10 and boron-11. Background Technology

[0002] Boron has two stable isotopes in nature, boron-10 and boron-11, with natural abundances of 19.78% and 80.22%, respectively. Both boron isotopes have extremely high application value. Boron-10 has a strong neutron absorption capacity with an absorption cross-section of 3837 target, and can be used as a neutron absorber in nuclear reactors, a gamma-ray shielding material, and a targeted drug in boron neutron capture therapy (BNCT). The "Guidance Catalogue for the First Batch of Application Demonstration of Key New Materials (2024 Edition)" specifies that the acid performance requirement for boron-10 is an abundance of ≥95%, and the drug efficacy in BNCT is controlled by the boron-10 abundance, with a preferred abundance of ≥99%. Boron-11 has extremely weak neutron absorption capacity, with an absorption cross-section of only 0.005 target. High-abundance boron-11, as a p-type doping source for silicon-based semiconductors, can be applied to various stages such as doping, oxidation diffusion, ion implantation, plasma etching, and silicon / germanium epitaxial growth. For example, precision processes in the semiconductor industry require high abundance and purity of electronic specialty gases such as boron trifluoride-11, with an abundance requirement of ≥99.8%. This broad application prospect correspondingly places high standards on the technology for separating boron isotopes.

[0003] Boron isotope separation methods include chemical exchange distillation, cryogenic distillation, extraction, adsorption separation, and laser methods. Chemical exchange distillation utilizes the different binding abilities of isotope molecules to form complexes with complexing agents to achieve separation; the separation coefficient of chemical exchange distillation is between 1.01 and 1.06. Cryogenic distillation utilizes the differences in the relative volatility of isotope molecules at low temperatures (-100°C) to achieve separation; the separation coefficient of cryogenic distillation for boron isotope separation is between 1.003 and 1.008. Extraction methods utilize the differences in the solubility of different isotope molecules by the extractant to achieve separation. Patent CN116726702A provides a method for the extraction and separation of boron isotopes. The hydrophobic deep eutectic solvent for boron isotopes uses diol compounds containing dihydroxyl groups as hydrogen bond donors and compounds containing phenolic hydroxyl groups or solid monohydric alcohols as hydrogen bond acceptors. The aqueous phase is an aqueous solution of boric acid, achieving separation coefficients ranging from 1.011 to 1.033. Adsorption separation methods can be divided into ion exchange resin adsorption and organometallic framework (MOF) adsorption. Patent CN116603391A invented a method for separating boron isotopes using DB564 or D403 resins, which can achieve separation by repeatedly adjusting the pH value of the boric acid aqueous solution. 10 B abundance was enriched to between 86-92%.

[0004] Although various separation methods are constantly being developed, extraction and resin adsorption, as efficient, energy-saving, and green processes, have high development prospects. However, these methods still suffer from problems such as low separation coefficients, complex operations, difficulties in industrial scale-up, and low yields. Currently, only chemical exchange distillation has achieved the industrial-scale separation and production of boron isotopes. The world's largest boron isotope producer is Serestan in the United States, which uses anisole-boron trifluoride chemical exchange distillation system, accounting for more than 85% of the world's total production at its peak. In addition, Italy's SCL and Japan's Stellachemifa have both achieved industrial-scale boron isotope separation using the anisole-boron trifluoride system. The industrial-scale separation of boron isotopes in China developed relatively late. Dalian Borntan achieved the industrial production of 96.5% boron-10 acid in 2009; subsequently, Liaoning Honghao achieved an annual production of 7 tons of boron-10 acid in 2016; and Shandong Heyi Gas Company developed an annual production of 1000 kg of boron-11 trifluoride in 2022. The key challenge in industrial production using chemical exchange distillation lies in ensuring yield while simultaneously increasing abundance, directly producing high-abundance, high-purity boron isotope products (boron-10 abundance greater than 99%, boron-11 abundance greater than 99.9%; corresponding product purity greater than 99%). The literature "Principles of Chemical Separation of Isotopes" and "Basic Chemistry and Applications of Isotopes" summarize the flow chart of the chemical exchange distillation process, as attached. Figure 1 As shown, the process is divided into three parts: exchange distillation, complexation, and cracking, which forms the basis of existing chemical exchange processes. The literature *Engineering-Scale Studies of Boron Isotope Separation* conducted bench tests on the enrichment of boron isotopes through chemical exchange distillation. The results presented in this literature showed that the maximum abundance of boron-10 was only 22%, and the maximum abundance of boron-11 was only 83%, far below the high abundance requirement. Patent CN102773016A discloses a multi-tower series boron isotope separation process, but the maximum abundance of boron-10 and boron-11 is only 95%, also failing to meet the high abundance requirement. Patents CN115920632A and CN115608156B innovated the complexation and cracking processes, respectively, improving the efficiency of the complexation and cracking reactions, but still did not completely solve the problem of simultaneously achieving high abundance of boron-10 and boron-11 after exchange distillation. In summary, there are no reports of separation processes for the co-production of high-abundance boron-10 and high-abundance boron-11. High-abundance boron-11 products, in particular, have never been found. Summary of the Invention

[0005] Analysis of existing chemical exchange distillation processes revealed that the cracking of the boron trifluoride-10-anisole complex is subject to chemical equilibrium limitations. Incomplete cracking inevitably results in boron-10 components being carried back to the complexation reactor in the anisole, severely impacting the boron-11 product abundance. Calculations show that only when the fraction of boron trifluoride-10-anisole complex in the post-cracking stream is less than 10 ppm will the boron-11 product abundance exceed 99.9%. This requires near-complete cracking of the complex.

[0006] Based on the above analysis, this invention provides a process and apparatus for high-quality boron isotope separation, particularly a process for the continuous production of high-grade boron-11 (99.9% abundance). The process utilizes naturally abundant boron trifluoride as feedstock. Building upon the existing exchange distillation, complexation, and cracking processes, a boron-11 refining system is employed to further enrich boron-11. The feedstock is the boron-11 enriched through the first-stage exchange distillation, which undergoes a second-stage chemical exchange distillation process. A deep cracker is used to completely decompose the boron-10 complex, further increasing the boron-11 abundance and simultaneously obtaining high-abundance boron-10 and boron-11 products. To achieve complete complex cracking, the deep cracker operates at a higher cracking temperature than all other cracking reactors, and operates under slight negative pressure.

[0007] The technical solution of the present invention is as follows:

[0008] A process for high-quality boron isotope separation includes an exchange distillation system, a complexation system, a complex cracking system, and a boron-11 purification system, wherein:

[0009] Exchange distillation system: After the temperature of the naturally abundant boron trifluoride feedstock is stabilized in the feed heat exchanger, it enters the boron-10 refining column from the middle and upper part of the column;

[0010] Complexation System: The overhead stream from the boron-10 refining tower enters the complexation reactor and complexes with anisole to form boron trifluoride-anisole complex. The gaseous product from the complexation reactor is collected as a high-abundance crude boron-11 product and removed from the boron-11 refining system. The liquid product from the complexation reactor is returned to the boron-10 refining tower as a cold-end liquid reflux via the boron-10 refining tower reflux pump.

[0011] Complex cracking system: The bottom stream of the boron-10 refining tower is pumped into the low-temperature cracking tower and its reboiler via a low-temperature cracking transfer pump for initial cracking. The liquid stream from the low-temperature cracking reboiler is pumped through the high-temperature cracking tower and its reboiler via a high-temperature cracking transfer pump for further cracking of the complex. The liquid stream exiting the high-temperature cracking reboiler is purified anisole, which is cooled by anisole cooler and then enters the complexation reactor to complex with boron trifluoride gas from the top of the boron-10 refining tower. The top stream from the low-temperature cracking tower is cooled by the low-temperature cracking tower condenser to obtain high-abundance boron trifluoride-10 gas phase. Part of it is collected as product, and part is returned to the bottom of the boron-10 refining tower as hot-end reflux. The gas streams from the low-temperature cracking tower reboiler and the high-temperature cracking tower are combined and sent to the bottom of the low-temperature cracking tower. The gas stream from the high-temperature cracking tower reboiler is returned to the high-temperature cracking tower.

[0012] In the boron-11 refining system, the gaseous product from the complexation reactor is sent to the bottom of the boron-11 refining tower for further refining. The overhead stream from the boron-11 refining tower enters the boron-11 complexation reactor. The gaseous stream from the boron-11 complexation reactor is collected as the refined high-abundance boron-11 product, while the liquid stream returns to the top of the boron-11 refining tower as a cold-end reflux. The complex stream from the bottom of the boron-11 refining tower is pumped by a boron-11 complex cryogenic cracking pump into the boron-11 complex cryogenic cracking tower and the reboiler of the boron-11 complex cryogenic cracking tower for preliminary cracking. The liquid stream from the reboiler of the boron-11 complex cryogenic cracking tower then passes through the boron-11 complex... The high-temperature cracking pump of the compound is sent to the high-temperature cracking tower of boron-11 complex and the reboiler of the high-temperature cracking tower of boron-11 complex to complete the further cracking of the complex. The liquid phase discharge stream from the reboiler of the high-temperature cracking tower of boron-11 complex enters the deep cracking reactor for deep impurity removal to remove impurities from the stream and obtain high-purity recycled anisole. The liquid phase stream from the deep cracking reactor returns to the boron-11 complexing reactor, and the gas phase stream is discharged. The overhead stream of the low-temperature cracking tower of boron-11 complex is partially discharged after being condensed and impurity removed by the condenser of the low-temperature cracking tower of boron-11 complex, and part of it is used as the hot gas phase reflux at the bottom of the boron-11 refining tower.

[0013] In the aforementioned exchange distillation system, the boron-10 purification column adopts a packed column structure to achieve gas-liquid countercurrent contact reaction. The top product of the column is a gas phase enriched with boron-11, and the bottom product is a liquid phase enriched with boron-10. The theoretical plate number of the boron-10 purification column is 312~378, the temperature is 23~27°C, and the reflux ratio is 108~192.

[0014] In the complexation system, the complexation reactor is a tubular reactor with a reaction temperature of 20~27°C and a pressure of 0.8~1.2 bara. The flow rate of the gaseous material enriched with boron trifluoride-11 from the complexation reactor is controlled at 83~92% of the total flow rate of boron trifluoride feed, and the concentration is controlled at 90~93%.

[0015] In the complex pyrolysis system described above, the low-temperature pyrolysis reaction temperature is 110~140°C, and the high-temperature pyrolysis reaction temperature is 160~180°C.

[0016] In the boron-11 refining system, the boron-11 refining tower adopts a packed tower structure with a theoretical plate number of 337-382 and a reflux ratio of 280-287. The deep pyrolysis reactor is a fixed-bed packed reactor with a reaction temperature of 169-183 °C and a pressure of 0.71-0.96 bara. The gas phase fraction of the deep pyrolysis reactor is controlled between 8% and 13%. The high-quality boron trifluoride-11 abundance extracted from the gas phase in the boron-11 complexation reactor is controlled at 99.9%, and the suitable extraction flow rate is 48-56% of the total boron trifluoride feed flow rate.

[0017] The recovery rate of boron trifluoride-10 enriched in the gas phase of the condenser of the low-temperature pyrolysis tower is 7%~15% based on the feed rate, and the concentration is controlled at 85~99%.

[0018] This high-quality boron isotope separation process includes a regeneration cycle for the raw materials boron trifluoride and anisole. Anisole enters the system from the complexation reactor and the boron-11 complexation reactor, reacting with boron trifluoride to form a complex. The complex stream then passes through a boron-10 purification tower and a boron-11 purification tower before entering the cracking system. It sequentially passes through a low-temperature cracking tower and a high-temperature cracking tower to obtain cracked anisole, which is then returned to the complexation reactor for recycling. The boron-11 purification system also includes a deep cracking reactor for further impurity removal and purification of the anisole. The liquid phase feed is returned to the complexing reactor via a heat exchanger to achieve recycling. Boron trifluoride feedstock enters the process from the boron-10 purification tower, where it exists in two forms: boron trifluoride gas and boron trifluoride-anisole complex. The gaseous boron trifluoride from the exchange distillation tower is transported to the complexing reaction to generate the boron trifluoride-anisole complex. After an isotope exchange reaction, the boron trifluoride-anisole complex enters the cracking system, where it is cracked into boron trifluoride and anisole. The pure boron trifluoride is returned to the exchange distillation tower as a gaseous recirculation at the bottom of the tower, completing the boron trifluoride material recycling process.

[0019] The waste flow rate discharged from the deep pyrolysis reactor is controlled at 340~500kmol / h, and circulating anisole is replenished accordingly.

[0020] This invention discloses an apparatus for a high-quality boron isotope separation process, comprising an exchange distillation system, a complexation system, a complex cracking system, and a boron-11 purification system. The exchange distillation system is characterized by a boron-10 purification column (T-101) as its main component; the complexation system's main equipment is a complexation reactor (R-201); the complex cracking system includes a low-temperature cracking column (T-301) and a high-temperature cracking column (T-302); the boron-11 purification system includes a boron-11 purification column (T-401), a boron-11 complexation reactor (R-401), a boron-11 complex low-temperature cracking column (T-402), a boron-11 complex high-temperature cracking column (T-403), and a deep cracking reactor (R-402); the connection sequence is as follows: the top pipeline of the boron-10 purification column (T-101) is connected to the complexation reactor... The complexing reactor (R-201) is connected to the bottom pipeline of the boron-10 refining tower (T-101), which is connected to the low-temperature cracking tower (T-301). The bottom pipeline of the low-temperature cracking tower (T-301) is connected to the high-temperature cracking tower (T-302), which is connected to the bottom pipeline of the high-temperature cracking tower (T-302). The bottom pipeline of the high-temperature cracking tower (T-302) is connected to the complexing reactor (R-201). The gas phase discharge of the complexing reactor (R-201) is connected to the boron-11 refining tower (T-401). The top pipeline of the boron-11 refining tower (T-401) is connected to the boron-11 complexing reactor (R-401). The bottom pipeline of the boron-11 refining tower (T-401) is connected in sequence to the low-temperature cracking tower (T-402) of boron-11 complex, the high-temperature cracking tower (T-403) of boron-11 complex, and the deep cracking reactor (R-402).

[0021] The specific explanation is as follows:

[0022] A process for high-quality boron isotope separation includes an exchange distillation system, a complexation system, a complex cracking system, and a boron-11 purification system, wherein each system is briefly described below:

[0023] Exchange distillation system: Naturally abundant boron trifluoride undergoes an exchange reaction with enriched boron trifluoride-11 complex, and the reaction equation is as follows.

[0024] 11 BF3·CH3OC6H5+ 10 BF3→ 10 BF3·CH3OC6H5+ 11 BF3

[0025] Complexation system: enriched by exchange distillation system 11 BF3 undergoes a complexation reaction with anisole, and the reaction equation is as follows.

[0026] 11 BF3+CH3OC6H5→ 11 BF3·CH3OC6H5

[0027] Complex cleavage system: 11 The thermal decomposition of BF3-anisole complex is shown in the following reaction equation.

[0028] 11 BF3·CH3OC6H5→ 11 BF3+CH3OC6H5

[0029] Boron-11 purification system: The initially enriched boron trifluoride-11 obtained from the exchange distillation system is further enriched to obtain high-abundance boron-11. The reaction equation is as follows.

[0030] 11 BF3·CH3OC6H5+ 10 BF3→ 10 BF3·CH3OC6H5+ 11 BF3

[0031] 11 BF3+CH3OC6H5→ 11 BF3·CH3OC6H5

[0032] 11 BF3·CH3OC6H5→ 11 BF3+CH3OC6H5

[0033] use Figure 1A specific description of a high-quality boron isotope separation apparatus includes an exchange distillation system, a complexation system, a complex cracking system, and a boron-11 purification system. The main component of the exchange distillation system is a boron-10 purification column (T-101). The main equipment of the complexation system is a complexation reactor (R-201). The complex cracking system includes a low-temperature cracking column (T-301) and a high-temperature cracking column (T-302). The boron-11 purification system includes a boron-11 purification column (T-401), a boron-11 complexation reactor (R-401), a low-temperature boron-11 complex cracking column (T-402), a high-temperature boron-11 complex cracking column (T-403), and a deep cracking reactor (R-402). The connection sequence is as follows: the top pipeline of the boron-10 purification column (T-101) is connected to the complexation reactor... The bottom pipeline of the boron-10 refining tower (T-101) is connected to the low-temperature cracking tower (T-301). The bottom pipeline of the low-temperature cracking tower (T-301) is connected to the high-temperature cracking tower (T-302). The bottom pipeline of the high-temperature cracking tower (T-302) is connected to the complexing reactor (R-201). The gas phase discharge of the complexing reactor (R-201) is connected to the boron-11 refining tower (T-401). The top pipeline of the boron-11 refining tower (T-401) is connected to the boron-11 complexing reactor (R-401). The bottom pipeline of the boron-11 refining tower (T-401) is connected in sequence to the low-temperature cracking tower (T-402) of boron-11 complex, the high-temperature cracking tower (T-403) of boron-11 complex, and the deep cracking reactor (R-402).

[0034] The material flow direction is as follows:

[0035] For the exchange distillation system, the naturally abundant boron trifluoride feedstock enters the boron-10 purification column (T-101) from the upper middle part after the temperature is stabilized by the feed heat exchanger (E-101). The exchange distillation column is a packed column structure and does not have a separate condenser and reboiler.

[0036] For the complexation system, the overhead stream (mainly the initially enriched boron-11 stream) from the boron-10 refining tower (T-101) enters the complexation reactor (R-201) to complex with anisole to form a boron trifluoride-anisole complex. The gaseous product from the complexation reactor is discharged from the boron-11 refining system as a high-abundance crude boron-11 product, while the liquid product from the complexation reactor (mainly the initially enriched boron trifluoride-11-anisole complex) is returned to the boron-10 refining tower (T-101) as a cold-end liquid reflux via the boron-10 refining tower reflux pump (P-201).

[0037] For the complex cracking system, the bottom stream (mainly enriched boron-10) from the boron-10 purification tower (T-101) is pumped by the low-temperature cracking transfer pump (P-101) into the low-temperature cracking tower (T-301) and the low-temperature cracking tower reboiler (E-302) for initial cracking. The liquid stream (mainly incompletely cracked complexes) from the low-temperature cracking reboiler (E-302) is pumped by the high-temperature cracking transfer pump (P-301) through the high-temperature cracking tower (T-302) and the high-temperature cracking tower reboiler (E-303) for further cracking. The liquid stream exiting the high-temperature cracking tower reboiler (E-303) is purified anisole, which is cooled by the anisole cooler (E-304) before entering... The complexation reactor (R-201) complexes with the boron trifluoride gas at the top of the boron-10 refining tower; the overhead stream of the low-temperature cracking tower (T-301) is cooled by the low-temperature cracking tower condenser (E-301) to obtain a high-abundance boron trifluoride-10 gas phase, part of which is collected as a product and part is returned to the bottom of the boron-10 refining tower (T-101) as a hot-end reflux; the gas phase streams (mainly enriched boron trifluoride-10) from the low-temperature cracking tower reboiler (E-302) and the high-temperature cracking tower (T-302) are combined and sent to the bottom of the low-temperature cracking tower (T-301); the gas phase stream (mainly enriched boron trifluoride-10) from the high-temperature cracking tower reboiler (E-303) is returned to the high-temperature cracking tower (T-302).

[0038] For the boron-11 refining system, the gaseous product from the complexing reactor (R-201) is sent to the bottom of the boron-11 refining tower (T-401) for refining. The overhead stream from the boron-11 refining tower (T-401) enters the boron-11 complexing reactor (R-401). The gaseous stream from the boron-11 complexing reactor (R-401) is extracted as the refined high-abundance boron-11 product, and the liquid stream returns to the top of the boron-11 refining tower (T-401) as a liquid cold-end reflux. The complex stream from the bottom of the boron-11 refining tower (T-401) is pumped by the boron-11 complex cryogenic cracking pump (P-401) into the boron-11 complex cryogenic cracking tower (T-402) and the boron-11 complex cryogenic cracking tower reboiler (E-402) for preliminary cracking. The liquid stream from the boron-11 complex cryogenic cracking tower reboiler (E-402) is then pumped by the boron-11 complex high-temperature cracking pump (P-403) to the boron-11 complex high-temperature cracking tower (T-402). The high-temperature cracking tower reboiler (E-403) of the boron-11 complex completes the further cracking of the complex. The liquid stream from the reboiler (E-403) enters the deep cracking reactor (R-402) for deep purification to remove impurities and obtain high-purity recycled anisole. The liquid stream from the deep cracking reactor (R-402) returns to the boron-11 complexing reactor (R-401), while the gas stream is vented. The overhead stream from the low-temperature cracking tower (T-402) of the boron-11 complex is partially vented after being condensed and purified by the condenser (E-401), and partially used as reflux at the hot end of the bottom of the boron-11 purification tower (T-401).

[0039] The process of this invention includes a regeneration cycle for the raw materials boron trifluoride and anisole. Anisole enters the system from the complexing reactor (R-201) and the boron-11 complexing reactor (R-401), reacting with boron trifluoride to form a complex. The complex stream then passes through the boron-10 purification tower (T-101) and the boron-11 purification tower (T-401) before entering the cracking system. It sequentially passes through a low-temperature cracking tower and a high-temperature cracking tower to obtain cracked anisole, which is then returned to the complexing reactor for recycling. The boron-11 refining system is additionally equipped with a deep cracking reactor (R-402) to remove impurities and purify anisole. The liquid phase output from the deep cracking reactor (R-402) is returned to the complexing reactor via a heat exchanger (E-404) for recycling. Boron trifluoride feedstock enters the process from the boron-10 refining tower (T-101), where it exists in two forms: boron trifluoride gas and boron trifluoride-anisole complex. The gaseous boron trifluoride from the exchange distillation tower is transported to the complexing reaction to generate the boron trifluoride-anisole complex. After an isotope exchange reaction, the boron trifluoride-anisole complex enters the cracking system, where it is cracked into boron trifluoride and anisole. The pure boron trifluoride is returned to the exchange distillation tower as a gaseous recirculation at the bottom of the tower, completing the material recycling of boron trifluoride.

[0040] The exchange distillation system of this invention consists of a boron-10 purification column (T-101), which adopts a packed column structure to achieve gas-liquid countercurrent contact reaction. The top product of the column is a boron-11 enriched gas phase, and the bottom product is a boron-10 enriched liquid phase. The suitable theoretical plate number of the boron-10 purification column (T-101) is 312~378. The isotope exchange temperature and reactivity in the column are jointly controlled by the return liquid phase temperature of the complexing reactor (R-201) and the return gas phase temperature of the low-temperature cracking column (T-301), and the suitable temperature is 23~27℃.

[0041] The complexation system of this invention consists of a complexation reactor (R-201), which is a tubular reactor. The gas phase feed to the reactor comes from the overhead stream of the boron-10 purification tower (T-101), and the liquid phase includes replenished fresh anisole and anisole decomposed from the high-temperature cracking tower (T-302) in the cracking system. The preferred reaction temperature is 20~27℃, and the pressure is 0.8~1.2 bara.

[0042] The complex cracking system of this invention consists of a low-temperature cracking tower (T-301), a low-temperature cracking tower reboiler (E-302), a high-temperature cracking tower reboiler (E-303), and a high-temperature cracking tower (T-302), both of which employ packed structures. The boron-10-enriched boron trifluoride-anisole complex produced from the bottom of the exchange distillation tower (T-101) serves as the feed stream, undergoing initial decomposition in the low-temperature cracking tower (T-301). The suitable temperature for the low-temperature cracking reaction is 110–140°C. Incompletely cracked complexes further enter the low-temperature cracking tower (T-302) for complete cracking, with a suitable temperature for the high-temperature cracking reaction of 160–180°C. The cracked gas, the product of the cracking system, is condensed and collected by the low-temperature cracking tower condenser (E-301).

[0043] The boron-11 refining system of this invention consists of a boron-11 refining tower (T-402), a boron-11 complexing reactor (R-401), a low-temperature cracking tower for boron-11 complexes (T-402), a high-temperature cracking tower for boron-11 complexes (T-403), and a deep cracking reactor (R-402). The boron-11 refining system uses the product of boron-11 initially enriched in the complexing reactor (R-201) of the complexing system as raw material. The boron-11 refining tower (T-401) then completes the enrichment of high-quality boron trifluoride. The boron-11 refining tower adopts a packed tower structure with bottom feeding, and a suitable theoretical plate number of 337~382. The top of the refining tower is equipped with a boron-11 complexation reactor to achieve liquid-phase circulation, and the bottom of the tower is equipped with a boron-11 complex cracking device, including a low-temperature cracking tower (T-402) for boron-11 complex, a high-temperature cracking tower (T-402) for boron-11 complex, and a deep cracking reactor (R-402). The deep cracking reactor (R-402) is a fixed-bed packed reactor to remove trace amounts of boron-10 impurities from the cracked anisole. The suitable reaction temperature of the deep cracking reactor (R-402) is 169~183℃, and the suitable pressure is 0.71~0.96 bara.

[0044] Preferably, the reflux ratio of the boron-10 refining column (T-101) is 108~192;

[0045] Preferably, the recovery rate of enriched boron trifluoride-10 is between 7% and 15% (based on feed rate);

[0046] Preferably, the boron-11 trifluoride recovery rate in the refined boron-11 system is between 48% and 56% (based on feed rate);

[0047] Preferably, in the refined boron-11 system, the gas phase fraction of the deep pyrolysis reactor (R-402) is controlled between 8% and 13%.

[0048] The beneficial technical effects of this invention are as follows:

[0049] 1. This invention uses boron trifluoride-anisole chemical exchange distillation to separate boron isotopes. Compared with extraction and resin adsorption methods, the process is shorter, the equipment is simpler, the operating conditions are more suitable, and the separation coefficient is higher, which can meet the requirements of industrial mass production.

[0050] 2. This invention connects the industrial processes of boron-10 refining and boron-11 refining, simultaneously achieving continuous production of two high-quality boron isotopes, greatly improving production efficiency. The abundance of boron-10 can reach 99%, and the abundance of boron-11 can reach 99.9%.

[0051] 3. This invention discovered that the main factor limiting the abundance of boron isotopes is the trace impurities remaining in the process. It innovatively uses a deep cracking reactor to control the trace impurities in the process. The boron-10 content in the top stream of the exchange distillation column returned to the boron-11 purification system is less than 0.01%, of which the boron trifluoride-10-anisole complex content is less than 10 ppm, thereby maximizing the abundance of boron-11. Attached Figure Description

[0052] Figure 1 This is a schematic diagram of the process flow for separating high-quality boron isotopes according to the present invention.

[0053] Among them: T-101—Boron-10 refining tower, T-301—Low-temperature cracking tower, T-302—High-temperature cracking tower, T-401—Boron-11 refining tower, T-402—Boron-11 complex low-temperature cracking tower, T-403—Boron-11 complex high-temperature cracking tower, R-201—Complexing reactor, R-401—Boron-11 complexing reactor, R-402—Deep cracking reactor;

[0054] E-101 – Feed heat exchanger, E-301 – Low-temperature cracking tower condenser, E-302 – Low-temperature cracking tower reboiler, E-303 – High-temperature cracking tower reboiler, E-304 – Anisole cooler, E-401 – Boron-11 complex low-temperature cracking tower condenser, E-402 – Boron-11 complex low-temperature cracking tower reboiler, E-403 – Boron-11 complex high-temperature cracking tower reboiler, E-404 – Circulating anisole cooler;

[0055] P-101 – Boiler pump from the boron-10 refining tower; P-201 – Feed pump from the complexation reactor; P-301 – Boiler pump from the low-temperature pyrolysis tower; P-302 – Boiler pump from the high-temperature pyrolysis tower; P-401 – Boiler pump from the boron-11 refining tower; P-402 – Feed pump from the boron-11 complexation reactor; P-403 – Boiler pump from the low-temperature pyrolysis tower of boron-11 complex; P-404 – Boiler pump from the high-temperature pyrolysis tower of boron-11 complex. Detailed Implementation

[0056] This invention provides a process and apparatus for high-quality boron isotope separation, particularly a process for the continuous production of high-grade boron-11 (99.9% abundance). The following is a description of the method and apparatus of this invention in conjunction with the accompanying drawings.

[0057] This invention is achieved through Figure 1 The method shown is implemented as follows:

[0058] The apparatus for boron isotope separation according to the present invention includes an exchange distillation system, a complexation system, a complex cracking system, and a boron-11 purification system. The exchange distillation system mainly includes a boron-10 purification column (T-101), which is connected to its auxiliary equipment, a feed heat exchanger (E-101) and a boron-10 purification column bottom pump (P-101).

[0059] The complexation system mainly includes a complexation reactor (R-201), which is connected to a boron-10 refining tower (T-101) via its auxiliary equipment, a complexation reactor discharge pump (P-201).

[0060] The pyrolysis system mainly includes a low-temperature pyrolysis tower (T-301) and a high-temperature pyrolysis tower (T-302). The low-temperature pyrolysis tower (T-301) is connected to its auxiliary equipment, namely the low-temperature pyrolysis tower condenser (E-301), the low-temperature pyrolysis tower reboiler (3E-302), and the low-temperature pyrolysis tower bottom pump (P-301). The high-temperature pyrolysis tower (T-302) is connected to its auxiliary equipment, namely the high-temperature pyrolysis tower reboiler (E-303), the high-temperature pyrolysis tower bottom pump (P-302), and the anisole cooler (E-303).

[0061] The boron-11 refining system mainly includes a boron-11 refining tower (T-401), a boron-11 complex low-temperature cracking tower (T-402), a boron-11 complex high-temperature cracking tower (T-403), a deep cracking reactor (R-402), and a boron-11 complexation reactor (R-401) connected in sequence. The boron-11 refining tower (T-401) is connected to the boron-11 complex low-temperature cracking tower (T-402) via its auxiliary equipment, a boron-11 refining tower bottom pump (P-401). The boron-11 complex low-temperature cracking tower (T-402) is connected to its auxiliary equipment, a boron-11 complex low-temperature cracking tower condenser (E-401). The boron-11 complex low-temperature cracking tower reboiler (E-402) and the boron-11 complex low-temperature cracking tower bottom discharge pump (P-403) are connected. The boron-11 complex high-temperature cracking tower (T-403) is connected to its auxiliary equipment, the boron-11 complex high-temperature cracking tower reboiler (E-403), the boron-11 complex high-temperature cracking tower bottom discharge pump (P-404), the deep cracking reactor (R-402), and the circulating anisole cooler (E-404). The boron-11 complexing reactor (R-401) is connected to the boron-11 refining tower (T-401) through its auxiliary equipment, the boron-11 complexing reactor discharge pump (P-402).

[0062] The high-quality boron isotope separation process described in this invention is as follows:

[0063] The boron-10 refining tower (T-101) is used to enrich boron-10 isotopes through a chemical exchange reaction. Naturally abundant boron trifluoride feedstock is fed from the middle of the tower, while a boron-11-rich liquid phase from the complexing reactor (R-201) is fed from the top of the tower, and a boron-10-rich gas phase from the low-temperature cracking tower (T-301) is fed from the bottom of the tower. Through the isotope exchange reaction, boron-11 isotopes are gradually enriched in the top gas phase of the tower. The boron-11 enriched gas phase at the top of the boron-10 refining tower serves as the feed stream for the complexing reactor (R-201). At the same time, boron-10 isotopes are gradually enriched in the bottom liquid phase of the tower. The bottom stream is sent to the low-temperature cracking tower (301) feed via the boron-10 refining tower bottom pump (P-101).

[0064] The complexation reactor (R-201) is used for complex regeneration and the extraction of high-quality boron trifluoride-10. The feed gas stream comes from the top of the boron-10 refining tower (T-101) with high abundance boron trifluoride-10, and the feed liquid stream comes from the bottom of the high-temperature cracking tower (T-302) with high purity anisole. Since the complexation reaction is a strongly exothermic reaction, the temperature of the complexation reactor (R-201) needs to be strictly controlled during the reaction process. The generated complex is sent to the boron-10 refining tower feed via the complexation reactor discharge pump (P-201). The gaseous product of the complexation reactor is sent to the boron-11 refining tower (T-401) as feed for the boron-11 refining system.

[0065] The low-temperature pyrolysis tower (T-301), the high-temperature pyrolysis tower (T-302), and their associated low-temperature pyrolysis tower reboiler (E-302) and high-temperature pyrolysis tower reboiler (E-303) are used to separate boron trifluoride from anisole, thereby achieving material recycling. The complex collected from the boron-10 refining tower (T-101) first enters the low-temperature cracking tower (T-301), where it exchanges heat with the mixed gas phase from the reboiler (T-301) and the top of the high-temperature cracking tower (T-302). Part of the complex is cracked here, and the rising gas phase, after initial cooling, exits the tower and passes through the low-temperature cracking tower condenser (E-301) to condense the anisole and boron trifluoride-anisole complex. The gas phase portion is collected as high-quality boron trifluoride-10 gaseous product, while the majority returns to the boron-10 refining tower (T-101) as bottom gas reflux, and the liquid phase returns to the low-temperature cracking tower (T-301). The bottom product of the low-temperature cracking tower (T-301) enters the reboiler (E-302) for further cracking. The reboiler is heated by steam, and the cracked boron trifluoride-10 gaseous product returns to the low-temperature cracking tower. The bottom of the low-temperature pyrolysis tower (T-301) serves as a gas-phase reflux and provides heat for pyrolysis within the tower. The liquid phase after passing through the reboiler of the low-temperature pyrolysis tower (E302) is pumped by the bottom pump of the low-temperature pyrolysis tower (P-301) to the feed of the high-temperature pyrolysis tower (T-302) for further pyrolysis. The top discharge of the high-temperature pyrolysis tower (T-302) is a gas-phase mixture of boron trifluoride and anisole, which is sent to the bottom of the low-temperature pyrolysis tower (T-301) for feed. The bottom discharge of the high-temperature pyrolysis tower (T-302) enters the reboiler of the high-temperature pyrolysis tower (E-303) to ensure sufficient pyrolysis. The gas-phase stream from the reboiler of the high-temperature pyrolysis tower (E-303) returns to the high-temperature pyrolysis tower (T-302) as a gas-phase reflux, while the liquid-phase stream is recycled anisole, which is sent by the bottom pump of the high-temperature pyrolysis tower (P-302) to the complexation reactor (R-201) for circulation.

[0066] The boron-11 refining tower (T-401) is used to refine boron trifluoride-11. The initially enriched boron trifluoride-11 is taken from the complexation reactor (R-201) and fed into the bottom of the refining tower. The boron-11 refining tower (T-401) adopts a packed tower structure and has only a rectification section. The enriched gas phase at the top of the boron-11 refining tower (T-401) is boron-11 product and is sent to the boron-11 complexation reactor (R-401). The bottom stream of the boron-11 refining tower (T-401) is sent to the boron-11 complex low-temperature cracking tower (T-402) by the bottom pump (P-401).

[0067] The boron-11 complexation reactor (R-401) is used to generate boron-11 complexes through a complexation reaction, enabling liquid-phase reflux at the top of the boron-11 purification column (T-401) and producing high-quality boron-11 trifluoride. The resulting liquid boron-11 complexes are pumped from the boron-11 complexation reactor to the top of the boron-11 purification column (T-401) for reflux by the feed pump (P-402).

[0068] The boron-11 complex low-temperature cracking tower (T-402), the boron-11 complex high-temperature cracking tower (T-403), the deep cracking reactor (R-402), and their auxiliary equipment, including the boron-11 complex low-temperature cracking tower condenser (E-401), the boron-11 complex low-temperature cracking tower reboiler (E-402), the boron-11 complex high-temperature cracking tower reboiler (E-403), and the circulating anisole cooler (E-404), are used to separate and enrich boron-11 boron trifluoride-anisole complexes. The bottom stream of the boron-11 refining tower (T-401) is pumped by the bottom pump (P-401) into the boron-11 complex low-temperature cracking tower (T-402) for cracking. The boron trifluoride gas phase from the top of the boron-11 complex low-temperature cracking tower (T-402) is condensed by the condenser (E-401). Part of the condensate is discharged as waste gas, and the rest is returned to the bottom of the boron-11 refining tower (T-401) as gas reflux. The bottom stream of the boron-11 complex low-temperature cracking tower (T-402) enters the reboiler (E-402) for further cracking. The gas phase from the reboiler (E-402) returns to the bottom of the boron-11 complex low-temperature cracking tower (T-402) as gas reflux. The liquid phase is pumped by the bottom pump (P-403) to the boron-11 complex high-temperature cracking tower (T-403) for further cracking. The high-temperature cracking tower (T-403) for boron-11 complex operates at a higher temperature than the low-temperature cracking tower (T-402) for boron-11 complex. The vapor stream from the top of the high-temperature cracking tower (T-403) returns to the bottom of the low-temperature cracking tower (T-402) as reflux. The liquid phase from the bottom enters the reboiler (E-403) for complete cracking. The vapor phase from the reboiler (E-403) returns to the boron-11 complex. The bottom of the low-temperature cracking tower (T-402) for complexing is used as a gas phase reflux. The liquid phase, due to the presence of trace impurities, is further sent to the deep cracking reactor (R-402) by the bottom pump (P-404) of the high-temperature cracking tower for boron-11 complexing to remove trace amounts of boron-10. The gas phase from the deep cracking reactor (R-402) is discharged as waste gas. The pure liquid anisole is cooled by the circulating anisole cooler (E-404) and then used as feed to the boron-11 complexing reactor (R-401).

[0069] In the first embodiment of the present invention, the feed abundance of boron trifluoride-10:boron trifluoride-11 is 19.78:80.22, the feed flow rate is 21.6 kmol / h, the theoretical number of plates of the boron-10 purification column (T-101) is 312, the feed is fed from the 177th plate, the complexation reactor (R-201) is kept at a constant reaction temperature of 23°C and a pressure of 1.0 bara, and the reflux ratio R back to the boron-10 purification column (T-101) is 192. The low-temperature cracking tower (T-301) is equipped with 10 theoretical plates. The condenser (E-301) of the low-temperature cracking tower has a condensation temperature of 25℃, and the reboiler (E-302) of the low-temperature cracking tower has a reboiling temperature of 110℃. The high-temperature cracking tower (T-302) is also equipped with 10 theoretical plates, and the reboiler (E-303) of the high-temperature cracking tower has a reboiling temperature of 174℃. The anisole cooler (E-304) is set to a temperature of 25℃. The boron trifluoride-10 effluent flow rate is 1.8 kmol / h, the abundance is 85%, and the process heating unit consumption is 164.98 Gcal / t. The boron-11 refining tower (T-401) has a theoretical plate count of 371, a feed abundance of 93%, and a reflux ratio of 287. The deep cracking reactor (R-402) has a reaction temperature of 183℃ and a pressure of 0.71 bara. The boron-11 complexing reactor (R-401) has an anisole flow rate of 402 kmol / h, a boron trifluoride-11 recovery abundance of 99.9%, a yield of 48%, and a heating consumption of 81.24 Gcal / t in the refining section.

[0070] In the second embodiment of the present invention, the feed flow rate of boron trifluoride is 21.6 kmol / h, the feed abundance of boron-10:boron-11 is 19.78:80.22, the theoretical number of plates of the boron-10 purification column (T-101) is 378, the feed is fed from the 210th plate, the complexation reactor (R-201) is kept at a constant reaction temperature of 20°C and a pressure of 1.2 bara, and the reflux ratio R of the boron-10 purification column (T-101) is 142. The low-temperature cracking tower (T-301) is equipped with 10 theoretical plates. The condenser (E-301) of the low-temperature cracking tower has a condensation temperature of 27℃, and the reboiler (E-302) of the low-temperature cracking tower has a reboiling temperature of 128℃. The high-temperature cracking tower (T-302) is also equipped with 10 theoretical plates, and the reboiler (E-303) of the high-temperature cracking tower has a reboiling temperature of 180℃. The anisole cooler (E-304) has a temperature set at 25℃. The boron trifluoride-10 effluent flow rate is 2.8 kmol / h, the abundance is 99%, and the process heating unit consumption is 177.20 Gcal / t. The boron-11 refining tower (T-401) has a theoretical plate count of 337, a feed abundance of 90%, and a reflux ratio of 277. The deep cracking reactor (R-402) has a reaction temperature of 183℃ and a pressure of 0.84 bara. The boron-11 complexing reactor (R-401) has a supplemental anisole flow rate of 340 kmol / h, a boron trifluoride-11 recovery abundance of 99.9%, a yield of 56%, and a heating consumption of 78.44 Gcal / t in the refining section.

[0071] As a third embodiment of the present invention, the feed flow rate of boron trifluoride is 21.6 kmol / h, the feed abundance of boron-10:boron-11 is 19.78:80.22, the theoretical number of plates of the boron-10 purification column (T-101) is 345, the feed is fed from the 196th plate, the complexation reactor (R-201) is kept at a constant reaction temperature of 27°C and a pressure of 0.8 bara, and the reflux ratio R of the boron-10 purification column (T-101) is 108. The low-temperature pyrolysis tower (T-301) is equipped with 10 theoretical plates. The condenser (E-301) of the low-temperature pyrolysis tower has a condensation temperature of 22℃, and the reboiler (E-302) of the low-temperature pyrolysis tower has a reboiling temperature of 140℃. The high-temperature pyrolysis tower (T-302) is also equipped with 10 theoretical plates, and the reboiler (E-303) of the high-temperature pyrolysis tower has a reboiling temperature of 160℃. The anisole cooler (E-304) is set to a temperature of 25℃. The boron trifluoride-10 effluent flow rate is 3.2 kmol / h, the abundance is 97%, and the process heating unit consumption is 340.38 Gcal / t. The boron-11 refining tower (T-401) has a theoretical plate count of 382, ​​a feed abundance of 91%, and a reflux ratio of 280. The deep cracking reactor (R-402) has a reaction temperature of 169℃ and a pressure of 0.96 bara. The boron-11 complexing reactor (R-401) has an anisole flow rate of 500 kmol / h, a boron trifluoride-11 recovery abundance of 99.9%, a yield of 53%, and a heating consumption of 80.42 Gcal / t in the refining section.

[0072] In one embodiment of the invention, the apparatus further includes a pump for conveying materials. As those skilled in the art will know, material conveying between the various distillation columns can utilize positional differences, relying on the gravity of the materials to achieve the conveying of raw materials within the distillation columns; however, when material conveying cannot be achieved by gravity, one or more material conveying pumps can be installed at appropriate pipeline locations to achieve material conveying.

[0073] Unless otherwise specified, the equipment used in this invention is conventional equipment, and can be implemented using methods and equipment known to those skilled in the art.

[0074] Although the invention has been described in conjunction with specific embodiments and accompanying drawings, it is not intended to be limited to the specific forms set forth herein. Rather, the scope of the invention is limited only by the appended claims. Furthermore, while individual features may be contained in different claims, these features may be advantageously combined, and inclusion in different claims does not imply that such combinations of features are not feasible and / or advantageous. References to "first," "second," etc., do not exclude the plural.

Claims

1. A process for high quality boron isotope separation, characterized in that, The system comprises an exchange rectification system, a complexing system, a complex cracking system and a boron-11 refining system, wherein: The exchange rectification system: the natural abundance boron trifluoride raw material is stabilized in temperature by a feed heat exchanger, and then enters the middle-upper part of the boron-10 refining column; The complexing system: the boron-10 refining column top stream is complexed with anisole in a complexing reactor to generate boron trifluoride-anisole complex, the complexing reactor gas phase product is taken out as high abundance boron-11 crude product to the boron-11 refining system, and the complexing reactor liquid phase product is taken back to the boron-10 refining column as a cold end liquid phase reflux through the boron-10 refining column reflux pump; The complex cracking system: the boron-10 refining column bottom stream is sent to the low-temperature cracking delivery pump to enter the low-temperature cracking column and the low-temperature cracking column reboiler to complete the preliminary cracking, the low-temperature cracking reboiler liquid phase stream is sent to the high-temperature cracking delivery pump to sequentially pass through the high-temperature cracking column and the high-temperature cracking column reboiler to complete the further cracking of the complex, the liquid phase stream from the high-temperature cracking column reboiler is the purified anisole, which is cooled by an anisole cooler and then enters the complexing reactor to be complexed with the boron-10 refining column top boron trifluoride gas; the low-temperature cracking column top stream is cooled by the low-temperature cracking column condenser to obtain the high abundance boron-10 gas phase, part of which is taken out as the product, and part of which is taken back to the boron-10 refining column bottom as a gas phase hot end reflux; the low-temperature cracking column reboiler and the high-temperature cracking column gas phase streams are combined and sent to the low-temperature cracking column bottom; the high-temperature cracking column reboiler gas phase stream is returned to the high-temperature cracking column; The boron-11 refining system: the complexing reactor gas phase product is sent to the bottom of the boron-11 refining column for refining, the boron-11 refining column top stream enters the boron-11 complexing reactor, the boron-11 complexing reactor gas phase stream is taken out as the refined high abundance boron-11 product, and the liquid phase stream is taken back to the boron-11 refining column top as a liquid phase cold end reflux; the boron-11 complex stream at the bottom of the boron-11 refining column is sent to the boron-11 complex low-temperature cracking pump to enter the boron-11 complex low-temperature cracking column and the boron-11 complex low-temperature cracking column reboiler for preliminary cracking, the boron-11 complex low-temperature cracking column reboiler liquid phase stream is sent to the boron-11 complex high-temperature cracking pump to the boron-11 complex high-temperature cracking column and the boron-11 complex high-temperature cracking column reboiler to complete the further cracking of the complex, the boron-11 complex high-temperature cracking column reboiler liquid phase outflow stream enters the deep cracking reactor to remove impurities in the outflow stream and obtain high purity circulating anisole, the deep cracking reactor liquid phase stream is taken back to the boron-11 complexing reactor, and the gas phase stream is exhausted; the boron-11 complex low-temperature cracking column top stream is condensed and impurities are removed by the boron-11 complex low-temperature cracking column condenser, part of which is exhausted, and part of which is taken as the boron-11 refining column bottom gas phase hot end reflux.

2. The process for high-quality boron isotope separation as described in claim 1, characterized in that, exchange... In the rectification system, the boron-10 refining column adopts a packed column structure to realize gas-liquid countercurrent contact reaction, the top product is a gas phase enriched with boron-11, and the bottom product is a liquid phase enriched with boron-10, the boron-10 refining column has a theoretical plate number of 312-378 and a temperature of 23-27℃, and the reflux ratio is 108-192.

3. The process for high quality separation of boron isotopes as claimed in claim 1 wherein, In the complexing system, the complexing reactor is a tube reactor, the reaction temperature is 20-27℃, and the pressure is 0.8-1.2 bara; the flow rate of the gas phase of the complexing reactor enriched in boron trifluoride-11 is controlled at 83-92% of the total flow rate of the boron trifluoride feed, and the concentration is controlled at 90-93%.

4. The process for high quality separation of boron isotopes as claimed in claim 1 wherein, In the complex decomposition system, the low-temperature decomposition reaction temperature is 110-140℃, and the high-temperature decomposition reaction temperature is 160-180℃.

5. The process for high quality separation of boron isotopes as claimed in claim 1 wherein, In the boron-11 refining system, the boron-11 refining column adopts a packed column structure, the theoretical plate number is 337-382, and the reflux ratio is 280-287; the deep decomposition reactor adopts a fixed bed packed reactor, the deep decomposition reactor reaction temperature is 169-183℃, the pressure is 0.71-0.96 bara; the gas phase fraction of the deep decomposition reactor is controlled at 8-13%; the high-quality boron trifluoride-11 enriched in the gas phase in the boron-11 complexing reactor is controlled at 99.9%, and the flow rate is 48-56% of the total flow rate of the boron trifluoride feed.

6. The process for high quality separation of boron isotopes as claimed in claim 1 wherein, The gas phase of the low-temperature decomposition column condenser is enriched in boron trifluoride-10, and the yield is 7-15% based on the feed amount, and the concentration is controlled at 85-99%.

7. The process for high quality separation of boron isotopes as claimed in claim 1 wherein, The process is provided with a regeneration cycle of the raw materials boron trifluoride and anisole; the raw material anisole enters the system from the complexing reactor and the boron-11 complexing reactor, reacts with boron trifluoride to generate a complex, and the complex stream passes through the boron-10 refining column and the boron-11 refining column, then enters the decomposition system, and is sequentially subjected to low-temperature decomposition and high-temperature decomposition to obtain decomposed anisole, and returns to the complexing reactor to realize circulation; the boron-11 refining system is additionally provided with a deep decomposition reactor to remove impurities and purify the anisole, and the liquid phase of the deep decomposition reactor is returned to the complexing reactor through a heat exchanger to realize circulation; the boron trifluoride raw material enters the process from the boron-10 refining column, exists in the process in the form of boron trifluoride gas and boron trifluoride-anisole complex, and the gas phase of the exchange rectification column is transported to the complexing reaction to generate boron trifluoride-anisole complex, the boron trifluoride-anisole complex is subjected to an isotopic exchange reaction, then enters the decomposition system, and is decomposed into boron trifluoride and anisole in the decomposition system, and the pure boron trifluoride returns to the exchange rectification column as the gas phase of the column bottom to complete the material circulation of boron trifluoride.

8. The process for high quality separation of boron isotopes as claimed in claim 7 wherein, The flow rate of the waste discharged from the deep decomposition reactor is controlled at 340-500 kmol / h, and the anisole is supplemented and circulated accordingly.

9. An apparatus for carrying out the process for high quality boron isotope separation as claimed in claim 1, comprising an exchange rectification system, a complexation system, a complex cleavage system and a boron-11 refining system; characterized in that, The main body of the exchange rectification system is a boron-10 refining tower (T-101); the main equipment of the complex system is a complex reactor (R-201); the complex cracking system comprises a low-temperature cracking tower (T-301) and a high-temperature cracking tower (T-302); the boron-11 refining system comprises a boron-11 refining tower (T-401), a boron-11 complex reactor (R-401), a boron-11 complex low-temperature cracking tower (T-402), a boron-11 complex high-temperature cracking tower (T-403) and a deep cracking reactor (R-402); the connection sequence is that a tower top pipeline of the boron-10 refining tower (T-101) is connected with the complex reactor (R-201), a tower bottom pipeline of the boron-10 refining tower (T-101) is connected with the low-temperature cracking tower (T-301), a tower bottom pipeline of the low-temperature cracking tower (T-301) is connected with the high-temperature cracking tower (T-302), a tower bottom pipeline of the high-temperature cracking tower (T-302) is connected with the complex reactor (R-201), a gas phase outlet of the complex reactor (R-201) is connected with the boron-11 refining tower (T-401), a tower top pipeline of the boron-11 refining tower (T-401) is connected with the boron-11 complex reactor (R-401), and a tower bottom pipeline of the boron-11 refining tower (T-401) is connected with the boron-11 complex low-temperature cracking tower (T-402), the boron-11 complex high-temperature cracking tower (T-403) and the deep cracking reactor (R-402) in sequence.

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