A method and system for efficiently separating boron isotopes
By establishing a circulation system for complexing, chemical exchange and cracking reactions during the separation of boron isotopes, and using the flow direction of the inert gas circulation gas to coincide with the reaction flow direction, the problems of high plate height and long equilibrium time in the prior art are solved, and the effect of efficient separation of boron isotopes is achieved.
Patent Information
- Application Number
- CN202410894453.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2023-11-17
- Filing Date
- 2024-07-04
- Publication Date
- 2025-04-18
- Estimated Expiration
- 2044-07-04
AI Technical Summary
In the prior art, the chemical exchange and rectification method of boron trifluoride-anisole complex requires a higher isoplastic height and a longer equilibrium time, resulting in low separation efficiency.
By establishing a cycle between complexation reaction, chemical exchange reaction and cleavage reaction, the complexation, exchange and cleavage reaction between anisole and 11BF3 and 10BF3 are gradually enriched, and the flow direction of the inert gas circulation gas is consistent with the reaction flow direction, thereby improving the mass transfer efficiency of the reaction.
The height of the isoplastic plates used in chemical exchange reactions and the equilibrium time of the system are reduced, the separation efficiency of boron isotopes is improved, and the efficient separation of boron isotopes is achieved.
Smart Images

Figure CN118681406B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a high-efficiency boron isotope separation method and system, belonging to the technical field of boron isotope separation. Background Art
[0002] The number of protons of the element boron is 5. Natural boron has two stable isotopes. The isotope with 5 neutrons is called boron 10 isotope (i.e. 10 B), the isotope with 6 neutrons is called boron 11 isotope (i.e. 11 B), natural boron 10 The abundance of B is 19.3%, 11 The abundance of B is 80.7%. The main reason for the rapid development of boron isotope separation is the huge difference in the absorption cross section of boron isotopes for thermal neutrons: 10 The absorption cross section of B for thermal neutrons is 3837 bar, while 11 B is only 0.005 bar, and the absorption cross section of natural abundance boron for thermal neutrons is close to 750 bar, so 10 The absorption cross section of boron for thermal neutrons is more than five times that of natural abundance boron. This characteristic is used as a control material for the stable operation of nuclear reactors, a radiation shielding material for nuclear reactors, a packaging material for the storage and transportation of hazardous waste, radiation protection for weapons and equipment, and targeted cancer treatment. 11 B can also be used in chip production.
[0003] At present, the methods for separating and enriching boron isotopes include: boron trifluoride chemical exchange distillation, boron trifluoride cryogenic distillation, boron trifluoride-sulfur dioxide cryogenic distillation, boric acid solution ion exchange, and boron trifluoride countercurrent circulation in series membranes. Boron trifluoride chemical exchange distillation is the main method for producing boron isotopes in the world. Boron trifluoride chemical exchange distillation has a high single-stage boron isotope separation coefficient and has reached industrial production scale.
[0004] Chemical exchange distillation mainly comprises boron trifluoride-ether complex chemical exchange distillation method, boron trifluoride-methyl ether complex chemical exchange distillation method and boron trifluoride-anisole complex chemical exchange distillation method.Boron fluoride-ether complex chemical exchange distillation method and boron trifluoride-methyl ether complex chemical exchange distillation method have been eliminated.The operating condition of boron trifluoride-anisole complex chemical exchange distillation method is normal temperature and pressure, and separation coefficient is high, raw material decomposition rate is low, toxicity is little, is the boron trifluoride chemical exchange distillation method commonly used in industry now, its separation coefficient can reach about 1.03, and anisole decomposition rate is within 0.1%.But boron trifluoride-anisole complex chemical exchange distillation method needs higher equal plate height to realize separation, needs long time from feeding to system balance. Summary of the invention
[0005] The purpose of the present invention is to provide a high-efficiency separation method for boron isotopes to solve the problems of high isoplate height and long equilibrium time required in the prior art boron trifluoride-anisole complex chemical exchange distillation method.
[0006] The second object of the present invention is to provide an efficient separation system for boron isotopes to solve the problems of high isoplate height and long equilibrium time required in the prior art chemical exchange distillation method of boron trifluoride-anisole complex.
[0007] In order to achieve the above purpose, the first technical solution of the present invention is:
[0008] An efficient separation method of boron isotopes, comprising sequentially cyclically performing complexation reaction, chemical exchange reaction and cleavage reaction;
[0009] Complexation reaction: anisole and 11 The BF3 enriched gas is subjected to complexation reaction to obtain a boron trifluoride·anisole complex liquid and an impurity-carrying inert gas, and the impurity-carrying inert gas is removed to obtain an inert gas circulation gas;
[0010] Chemical exchange reaction: Boron trifluoride·anisole complex liquid and mixed gas undergo chemical exchange reaction to obtain the 11 BF3 enriched gas and 10 BF3 enriched complex liquid; the mixed gas is composed of the inert gas circulating gas and 10 BF3 enriched gas composition;
[0011] Cleavage reaction: 10 The BF3-enriched complex solution is cracked to obtain the 10 BF3 enriched gas and crude anisole; crude anisole returned to the complexation reaction link after impurity removal and 11 BF3 enriched gas performs the complex reaction;
[0012] Detection 11 BF3 enriched gas 11 BF3 abundance and / or 10 BF3 enriched gas 10 BF3 abundance, until 11 BF3 abundance and / or 10 The BF3 abundance meets the requirements.
[0013] The present invention establishes a cycle between complex reaction, chemical exchange reaction and cracking reaction, so that the boron trifluoride 11 BF3, 10 BF3 and anisole continuously undergo complexation, exchange and cleavage, which makes the natural abundance of boron trifluoride 11 BF3 and 10 BF3 gradually enriched, thereby increasing11 BF3 and 10 The present invention also circulates an inert gas circulation gas between the chemical exchange reaction and the complex reaction, so that the flow direction of the inert gas circulation gas is consistent with that of the inert gas circulation gas. 10 BF3 enriched gas in chemical exchange reaction, 11 The flow direction of the BF3 enriched gas in the complex reaction is consistent, which improves the mass transfer efficiency of the reaction, thereby reducing the plate height used in the chemical exchange reaction, shortening the system equilibrium time, and achieving efficient separation of boron isotopes.
[0014] 11 BF3 enriched gas refers to the gas obtained by exchange enrichment through chemical exchange reaction. 11 BF3 gas and inert gas cycle gas, also refers to the natural abundance of boron trifluoride obtained after exchange enrichment 11 BF3 gas and inert gas circulation gas.
[0015] In order to further improve the separation efficiency, preferably, the volume ratio of the inert gas cycle gas to the boron trifluoride gas is (0.01-0.15):1; the boron trifluoride gas is 11 BF3 and 10 The boron trifluoride gas here refers to the natural abundance boron trifluoride gas to be separated.
[0016] In order to save costs, preferably, the inert gas is one or more of nitrogen, helium, and argon. These inert gases are conventional choices. Since any one of nitrogen, helium, and argon as an inert gas can improve the efficiency of separating boron isotopes, and the three have the same working principle, any two or three mixtures as an inert gas can still achieve the same technical effect.
[0017] In order to improve the separation efficiency and further improve the utilization rate of raw materials, preferably, the molar ratio of anisole to boron trifluoride gas is 1: (0.9-1.1); the boron trifluoride gas is 11 BF3 and 10 The sum of BF3.
[0018] In order to make the gas and liquid fully contact during the reaction and improve the reaction efficiency, preferably, the complexation reaction is carried out in a gas-liquid countercurrent form; the chemical exchange reaction is carried out in a gas-liquid countercurrent form. Preferably, in the gas-liquid countercurrent form, the gas moves upward and the liquid moves downward to carry out countercurrent contact. This can greatly reduce energy consumption.
[0019] In order to improve the cracking efficiency of the cracking reaction, preferably, the temperature of the cracking reaction is 150-160°C.
[0020] Preferably, the temperature of the complexation reaction is 20-35° C. and the pressure is 30-50 kPa. The complexation reaction can occur at room temperature and pressure, and the conditions are mild and convenient for reaction.
[0021] In order to facilitate the exchange and enrichment of boron isotopes, preferably, the temperature of the chemical exchange reaction is 20-35° C. and the pressure is 50-80 kPa. 11 BF3·anisole complex solution and 10 BF3 enriched gas is exchanged and enriched through chemical exchange reaction, so that 11 BF3 is enriched in the gas phase, 10 BF3 is enriched in the liquid phase.
[0022] The second technical solution of the present invention is:
[0023] A high-efficiency separation system for boron isotopes, comprising a complexing module, a chemical exchange module and a cracking module;
[0024] The complexation module is provided with an anisole inlet, 11 BF3 enriched gas inlet, first complexing liquid outlet and impurity-carrying inert gas outlet, the chemical exchange module is provided with a first complexing liquid inlet, 11 BF3 enriched gas outlet, mixed gas inlet and second complex liquid outlet, the cracking module is provided with a second complex liquid inlet, 10 BF3 enriched gas outlet and anisole crude product outlet;
[0025] The crude anisole product outlet is connected to the anisole impurity removal module, the anisole impurity removal module has a purified anisole outlet, and the purified anisole outlet is connected to the anisole inlet on the complexing module;
[0026] The impurity-carrying inert gas outlet is connected to the cooling and impurity removal module, and the cooling and impurity removal module has an inert gas circulation gas outlet;
[0027] The complexation module 11 BF3 enriched gas inlet and chemical exchange module 11 The BF3 enriched gas outlet is connected, the first complex liquid outlet on the complexing module is connected to the first complex liquid inlet on the chemical exchange module, the second complex liquid outlet on the chemical exchange module is connected to the second complex liquid inlet on the cracking module, the mixed gas inlet on the chemical exchange module is connected to the inert gas circulation gas outlet on the cooling and impurity removal module, the 10 The BF3 enriched gas outlet is connected.
[0028] The present invention forms a closed reaction loop between the complexation module, the chemical exchange module and the cracking module, which can improve the 10 BF3, 11The abundance of BF3 and 10 Inert gas circulation gas is introduced in parallel with BF3 enriched gas, so that the inert gas can continuously circulate between the chemical exchange module and the complexation module and participate in the reaction, thereby improving the mass transfer efficiency of the reaction, thereby reducing the height of the isoplate used for chemical exchange, shortening the system equilibrium time, and achieving efficient separation of boron isotopes.
[0029] In order to facilitate the feeding of anisole, preferably, the efficient boron isotope separation system comprises an anisole feeding area, and the anisole feeding area is arranged on the connecting pipe between the purified anisole outlet and the anisole inlet.
[0030] In order to facilitate the feeding of boron trifluoride, preferably, the chemical exchange module is connected to a boron trifluoride raw material area for supplying the boron trifluoride raw material to be separated into the separation system. The boron trifluoride raw material is boron trifluoride gas of natural abundance, wherein: 10 The abundance of BF3 is 19.3%, 11 The abundance of BF3 is 80.7%.
[0031] In order to facilitate the collection of 10 BF3 enriched gas, preferably, the cracking module is connected to 10 BF3 enriched gas refining area is used to collect 10 BF3 abundance requirement 10 BF3 enriched gas.
[0032] In order to facilitate the collection of 11 BF3 enriched gas, preferably, the chemical exchange module is connected to 11 BF3 enriched gas refining area is used to collect 11 BF3 abundance requirement 11 BF3 enriched gas.
[0033] Preferably, when 10 When the abundance of BF3 enriched gas reaches the preset requirement, the cracking module is turned on. 10 The passage between the BF3 enriched gas refining zone. 11 When the abundance of BF3 enriched gas reaches the preset requirement, the chemical exchange module is opened and 11 Passage between BF3 enriched gas refining zones.
[0034] Preferably, the temperature of the cooling and impurity removal module is -85° C. to -100° C. In this temperature range, the removal effect of impurities carried by the raw materials is better. BRIEF DESCRIPTION OF THE DRAWINGS
[0035] Figure 1 This is a diagram of the efficient separation system of boron isotopes in Example 1 of the present invention. DETAILED DESCRIPTION
[0036] The high-efficiency separation method of boron isotopes of the present invention comprises the following steps: cyclically carrying out complexation reaction, chemical exchange reaction and cleavage reaction; anisole and 11 After the BF3 enriched gas undergoes complexation reaction, a boron trifluoride·anisole complex liquid and an impurity-carrying inert gas are obtained. After the impurity-carrying inert gas is removed, an inert gas circulating gas is obtained to participate in the cycle. The boron trifluoride·anisole complex liquid continues to react with 10 BF3 enriched gas undergoes chemical exchange enrichment reaction, 11 BF3 is enriched in the gas phase. 10 BF3 is enriched in the liquid phase, where 10 The BF3 enriched gas is mixed with inert gas circulating gas. 10 BF3 is enriched in the liquid phase and then cracked to obtain 10 BF3 enriched gas and anisole, 10 The BF3 enriched gas refluxes to participate in the chemical exchange reaction again, and the anisole refluxes to participate in the complexation reaction again, thereby forming a reaction loop. In the present invention, an inert gas circulation gas is circulated between the complexation reaction and the chemical exchange reaction, which can further improve the mass transfer efficiency of the reaction, shorten the equilibrium time, and thus improve the separation efficiency of boron isotopes.
[0037] The reaction formula of the chemical exchange reaction involved in the present invention is as follows:
[0038]
[0039] The purity of the inert gas used in the following examples is greater than 99.999%; the water content of anisole is less than 10ppm and the purity is greater than 99.9%; boron trifluoride ( 11 BF3, 10 The water content of BF3 is less than 10ppm, the HF content is less than 15ppm, and the purity is greater than 99.9%.
[0040] The technical solution of the present invention is further described below in conjunction with specific implementation methods.
[0041] 1. The specific embodiments of the high-efficiency separation system of boron isotopes of the present invention are as follows:
[0042] Example 1
[0043] The efficient separation system of boron isotopes of this embodiment is as follows: Figure 1 As shown, it includes a complexing zone, a chemical exchange zone, a cracking zone, an anisole impurity removal zone and a cooling impurity removal zone, which correspond to the complexing module, the chemical exchange module, the cracking module, the anisole impurity removal module and the cooling impurity removal module respectively;
[0044] The complexation zone is equipped with an anisole inlet, 11BF3 enriched gas inlet, first complexing liquid outlet and impurity-carrying inert gas outlet are provided on the chemical exchange zone. 11 BF3 enriched gas outlet, mixed gas inlet and second complex liquid outlet, the cracking zone is provided with a second complex liquid inlet, 10 BF3 enriched gas outlet and anisole crude product outlet;
[0045] The crude anisole product outlet is connected to the anisole impurity removal zone, the anisole impurity removal zone has a purified anisole outlet, and the purified anisole outlet is connected to the anisole inlet on the complexing zone;
[0046] The impurity-carrying inert gas outlet is connected to the cooling and impurity removal zone, the cooling and impurity removal zone has an inert gas circulation gas outlet and an impurity outlet, and the impurity outlet is connected to the impurity treatment zone;
[0047] On the complexation zone 11 BF3 enriched gas inlet and chemical exchange zone 11 The BF3 enriched gas outlet is connected to the chemical exchange zone to 11 The BF3-enriched gas is transferred to the complexing zone, and the first complexing liquid outlet on the complexing zone is connected to the first complexing liquid inlet on the chemical exchange zone, so that the boron trifluoride·anisole complex produced in the complexing zone flows into the chemical exchange zone, and the second complexing liquid outlet on the chemical exchange zone is connected to the second complexing liquid inlet on the cracking zone, so that the boron trifluoride·anisole complex produced in the chemical exchange zone flows into the cracking zone for cracking to generate 10 BF3 enriched gas and anisole crude product, the mixed gas inlet on the chemical exchange zone and the inert gas circulating gas on the cooling and impurity removal zone, the 10 The BF3 enriched gas outlet is connected to facilitate the production of cracking zone 10 The BF3-enriched gas is mixed with the inert gas circulating gas from the cooling and impurity removal zone and enters the chemical exchange zone for reaction.
[0048] The chemical exchange zone is also connected to a boron trifluoride raw material zone for supplying the boron trifluoride raw material to be separated into the separation system. An anisole feeding zone is provided on the connecting pipeline between the purified anisole outlet and the anisole inlet. 10 BF3 enriched gas refining area is used to collect 10 BF3 abundance requirement 10 BF3 enriched gas; the chemical exchange zone is connected to 11 BF3 enriched gas refining area is used to collect 11 BF3 abundance requirement 11 BF3 enriched gas is further separated into the required 11 BF3.
[0049] 2. The specific embodiments of the efficient separation method of boron isotopes of the present invention are as follows:
[0050] Example 2
[0051] The efficient separation method of boron isotopes in this embodiment sequentially cycles through complexation reaction, chemical exchange reaction and cleavage reaction:
[0052] Complexation reaction: Anisole liquid and boron trifluoride gas (molar ratio 0.9:1) that meet the standards are placed in a complexation zone (20°C, 30 kPa) to form a boron trifluoride-anisole complex; the boron trifluoride gas is initially at natural abundance (e.g. Figure 1 In the chemical exchange zone, natural abundance boron trifluoride gas is introduced as the initial boron trifluoride gas. As the chemical exchange reaction occurs, 11 BF3 is continuously enriched.
[0053] Chemical exchange reaction: With the assistance of argon, the countercurrent mixed gas is exchanged with the boron trifluoride anisole complex in the exchange enrichment zone (20°C, 50kPa). 11 BF3 is enriched in the gas phase, 10 BF3 is enriched in the liquid phase. The gas mixture here contains argon and the 10 BF3 is a boron trifluoride gas that is continuously enriched.
[0054] Fragmentation reaction: leaving the exchange-enriched zone 10 The BF3·anisole liquid complex was pumped into the cracking zone and cracked by microwave heating (150°C). 10 BF3 enriched gas and crude anisole; 10 The BF3 enriched gas rises upward through the gas cooler, merges with the argon circulating gas after cooling and impurity removal, and enters the exchange enrichment zone together, and then enters the complexing tower; at the same time, the cracked anisole is pumped into the anisole impurity removal zone (heating with thermal oil) for rectification and impurity removal, and the impurity-removed anisole passes downward through the heat exchanger and is pumped to the top of the complexing zone; in the complexing zone, 11 BF3 and anisole are complexed and then continuously pumped to the top of the exchange enrichment zone. The argon gas carrying the impurity gas leaves the top of the complexation zone and enters the cooling and impurity removal zone (-85°C) to remove the impurity gas and then re-enters the exchange enrichment zone. The system enters total reflux.
[0055] After a period of time, the system reaches equilibrium. The volume ratio of argon to boron trifluoride circulating gas is 0.05:1, and the equilibrium time is 45h. 11 BF3 abundance is 99.69%, 10 The BF3 abundance is 95.68%.
[0056] Example 3
[0057] The efficient separation method of boron isotopes in this embodiment sequentially cycles through complexation reaction, chemical exchange reaction and cleavage reaction:
[0058] Complexation reaction: Standard anisole liquid and boron trifluoride gas (molar ratio 1.1:1) are placed in a complexation zone (35°C, 30 kPa) to form a boron trifluoride anisole complex; the boron trifluoride gas is initially in natural abundance, and as the chemical exchange reaction occurs, 11 BF3 is continuously enriched.
[0059] Chemical exchange reaction: With the assistance of argon, the countercurrent 10 BF3 gas is exchanged with boron trifluoride·anisole complex in the exchange enrichment zone (35°C, 50kPa). 11 BF3 is enriched in the gas phase, 10 BF3 is enriched in the liquid phase. The gas mixture here contains argon and the 10 BF3 is a boron trifluoride gas that is continuously enriched.
[0060] Fragmentation reaction: leaving the exchange-enriched zone 10 The BF3·anisole liquid complex is pumped into the cracking zone and is heated and cracked by heat transfer oil (160°C). The complex dissociates into 10 BF3 and anisole; 10 BF3 gas rises upward through the gas cooler, merges with the argon circulating gas after cooling and impurity removal, enters the exchange enrichment zone together, and then enters the complexing tower; at the same time, the cracked anisole is pumped into the anisole impurity removal zone (heating with thermal oil) for rectification and impurity removal, and the anisole after impurity removal passes downward through the heat exchanger and is pumped to the top of the complexing zone; in the complexing zone, 11 BF3 and anisole are complexed, and then continuously pumped to the top of the exchange enrichment zone. The argon gas carrying impurity gas leaves the top of the complexation zone and enters the cooling and impurity removal zone (-100℃) to remove the impurity gas and then re-enters the exchange enrichment zone. The system enters total reflux. The volume ratio of nitrogen to boron trifluoride circulating gas is 0.15:1.
[0061] Embodiment 4-11
[0062] The efficient separation method of boron isotopes in this embodiment sequentially cycles through complexation reaction, chemical exchange reaction and cleavage reaction:
[0063] Complexation reaction: standard anisole liquid and boron trifluoride gas (molar ratio 1:1) are placed in a complexation zone (25°C, 50 kPa) to form a boron trifluoride anisole complex; the boron trifluoride gas is initially in natural abundance, and as the chemical exchange reaction occurs, 11 BF3 is continuously enriched.
[0064] Chemical exchange reaction: With the assistance of inert gas, the countercurrent 10 BF3 gas is exchanged with boron trifluoride·anisole complex in the exchange enrichment zone (25°C, 80kPa). 11 BF3 is enriched in the gas phase, 10 BF3 is enriched in the liquid phase. The gas mixture here contains argon and the 10 BF3 is a boron trifluoride gas that is continuously enriched.
[0065] Fragmentation reaction: leaving the exchange-enriched zone 10 The BF3·anisole liquid complex was pumped into the cracking zone and cracked by microwave heating (150°C). 10 BF3 and anisole; 10 BF3 gas rises upward through the gas cooler, merges with the inert gas circulating gas after cooling and impurity removal, enters the exchange enrichment zone together, and then enters the complexing tower; at the same time, the cracked anisole is pumped into the anisole impurity removal zone (heating with thermal oil) for rectification and impurity removal, and the anisole after impurity removal passes downward through the heat exchanger and is pumped to the top of the complexing zone; in the complexing zone, 11 BF3 and anisole are complexed and then continuously pumped to the top of the exchange enrichment zone. The inert gas carrying impurities leaves the top of the complexation zone and enters the cooling and impurity removal zone (-95°C) to remove the impurities before re-entering the exchange enrichment zone. The system enters total reflux. After a period of time, the system reaches equilibrium.
[0066] The types and amounts of inert gases used in Examples 4-11 are shown in Table 1.
[0067] Table 1 Type and amount of inert gas in each example
[0068] Example Inert gas (5N) Volume ratio 4 Helium 0.05:1 5 Argon 0.05:1 6 Nitrogen 0.05:1 7 Argon 0.01:1 8 Argon 0.02:1 9 Argon 0.1:1 10 Nitrogen 0.1:1 11 Helium 0.1:1
[0069] 3. Comparison
[0070] Comparative Example 1
[0071] The boron isotope separation method of this comparative example is basically the same as that of Example 3, except that no inert gas is introduced.
[0072] IV. Experimental Examples
[0073] In this experimental example, the abundance and equilibrium time of boron isotopes obtained by the boron isotope separation method of Examples 2-11 and Comparative Example 1 were measured, and the results are shown in Table 2. The equilibrium time is from the end of feeding to 10 BF3, 11 The time when the abundance of BF3 no longer changes.
[0074] The abundance of boron isotopes was determined by ICP-MS (inductively coupled plasma-mass spectrometry).
[0075] Table 2 Results of determination of abundance and equilibrium time of boron isotopes
[0076] <![CDATA[ 11 BF3 abundance (%)]]> <![CDATA[ 10 BF3 abundance (%)]]> Equilibrium time Example 2 99.69 95.68 45h Example 3 98.99 89.01 35h Example 4 99.72 95.33 38h Example 5 99.73 96.01 37.5h Example 6 99.69 95.56 37.7h Example 7 97.01 60.23 65h Example 8 97.79 75.62 60h Example 9 98.95 85.54 30h Example 10 99.03 88.67 33h Embodiment 11 99.12 90.15 36h Comparative Example 1 96.32 38.65 72h
[0077] According to the measurement results in Table 2, compared with the comparative example 1 in which the inert gas is not introduced, the boron isotope separation method of the embodiment of the present invention can simultaneously improve 11 BF3 and 10 BF3 abundance, and can reduce system equilibrium time and improve separation efficiency.
Claims
1. A method for efficiently separating boron isotopes, characterized in that: It includes sequentially cyclically carrying out complexation reaction, chemical exchange reaction and cleavage reaction; Complexation reaction: anisole and 11 The BF3 enriched gas is subjected to complexation reaction to obtain a boron trifluoride·anisole complex liquid and an impurity-carrying inert gas, and the impurity-carrying inert gas is removed to obtain an inert gas circulation gas; Chemical exchange reaction: Boron trifluoride·anisole complex liquid and mixed gas undergo chemical exchange reaction to obtain the 11 BF3 enriched gas and 10 BF3 enriched complex liquid; the mixed gas is composed of the inert gas circulating gas and 10 The inert gas cycle gas is circulated between the chemical exchange reaction and the complex reaction; the volume ratio of the inert gas cycle gas to the boron trifluoride gas is (0.01-0.15):1; the boron trifluoride gas is 11 BF3 and 10 The sum of BF3; Cleavage reaction: 10 The BF3-enriched complex solution is cracked to obtain the 10 BF3 enriched gas and crude anisole; crude anisole returned to the complexation reaction link after impurity removal and 11 BF3 enriched gas performs the complex reaction; Detection 11 BF3 enriched gas 11 BF3 abundance and / or 10 BF3 enriched gas 10 BF3 abundance, until 11 BF3 abundance and / or 10 The BF3 abundance meets the requirements.
2. The method for efficiently separating boron isotopes according to claim 1, characterized in that: The inert gas is one or more of nitrogen, helium and argon.
3. The efficient separation method of boron isotopes according to claim 1, characterized in that: The molar ratio of anisole to boron trifluoride gas is 1:(0.9-1.1); the boron trifluoride gas is 11 BF3 and 10 The sum of BF3.
4. The method for efficiently separating boron isotopes according to claim 1, characterized in that: The complexation reaction is carried out in a gas-liquid countercurrent manner; and the chemical exchange reaction is carried out in a gas-liquid countercurrent manner.
5. A high-efficiency separation system of boron isotopes, used for a high-efficiency separation method of boron isotopes as claimed in any one of claims 1 to 4, characterized in that: It includes a complexation module, a chemical exchange module and a cracking module; The complexation module is provided with an anisole inlet, 11 BF3 enriched gas inlet, first complexing liquid outlet and impurity-carrying inert gas outlet, the chemical exchange module is provided with a first complexing liquid inlet, 11 BF3 enriched gas outlet, mixed gas inlet and second complex liquid outlet, the cracking module is provided with a second complex liquid inlet, 10 BF3 enriched gas outlet and anisole crude product outlet; The crude anisole product outlet is connected to the anisole impurity removal module, the anisole impurity removal module has a purified anisole outlet, and the purified anisole outlet is connected to the anisole inlet on the complexing module; The impurity-carrying inert gas outlet is connected to the cooling and impurity removal module, and the cooling and impurity removal module has an inert gas circulation gas outlet; The complexation module 11 BF3 enriched gas inlet and chemical exchange module 11 The BF3 enriched gas outlet is connected, the first complex liquid outlet on the complexing module is connected to the first complex liquid inlet on the chemical exchange module, the second complex liquid outlet on the chemical exchange module is connected to the second complex liquid inlet on the cracking module, the mixed gas inlet on the chemical exchange module is connected to the inert gas circulation gas outlet on the cooling and impurity removal module, the 10 The BF3 enriched gas outlet is connected.
6. The efficient separation system of boron isotopes according to claim 5, characterized in that: The high-efficiency boron isotope separation system comprises an anisole feeding area, and the anisole feeding area is arranged on a connecting pipeline between a purified anisole outlet and an anisole inlet.
7. The efficient separation system of boron isotopes according to claim 5, characterized in that: The chemical exchange module is connected to a boron trifluoride raw material zone for supplying the boron trifluoride raw material to be separated into the separation system.
8. The efficient separation system of boron isotopes according to claim 5, characterized in that: The cracking module is connected to 10 BF3 enriched gas refining area is used to collect 10 BF3 abundance requirement 10 BF3 enriched gas.
9. The efficient separation system of boron isotopes according to claim 5, characterized in that: The chemical exchange module is connected to 11 BF3 enriched gas refining area is used to collect 11 BF3 abundance requirement 11 BF3 enriched gas.
Citation Information
Patent Citations
Construction method based on technology for producing boron isotope by anisole-boron trifluoride
CN104190256A
Method for industrial production of boron isotope products
CN104209001A