CN113387368A - Production method of high-abundance boron-11 isotope - Google Patents
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Abstract
The invention relates to a production method of a high-abundance boron-11 isotope, which is characterized in that boron trifluoride is continuously fed from the bottom of a gas-liquid exchange device, complexing agent capable of carrying out complexing reaction with boron trifluoride raw material continuously enters from the top and the middle of the gas-liquid exchange device, so that the boron trifluoride and the complexing agent are in countercurrent contact in the gas-liquid exchange device, and a product rich in boron-11 is continuously extracted from a top outlet and/or a middle outlet of the gas-liquid exchange device. Compared with the prior art, the invention adopts a unique single-tower process, simplifies the prior complex processes of series connection and cascade connection, greatly improves the production stability, simultaneously improves the enrichment efficiency of boron-11, reduces the energy consumption, and can produce boron-11 isotopes with the abundance of 99.9 percent or more.
Description
Technical Field
The invention belongs to the technical field of isotope separation, and relates to a production method of a high-abundance boron-11 isotope.
Background
Due to the lack of atmospheric protection, spacecraft integrated chips are susceptible to bombardment by high energy particles, the most significant of which is the single particle effect. It is reported in the united states that half of satellite failures are due to this effect. The single event effect means that after single high-energy particles (such as heavy ions, protons, neutrons and the like) in a space radiation environment are incident into an integrated chip, impact electrons form free electron pairs, and when the impact electrons reach a certain number, the logic state of a circuit is overturned, and even the circuit fails.
In nature, boron has two stable isotopes, boron-10 and boron-11, at 19.8 ± 0.2% and 80.2% ± 0.2% respectively. Boron-10 has a large thermal neutron absorption cross section, and boron-11, on the contrary, hardly absorbs neutrons, so that the boron-10 is mainly used as a dopant in the manufacturing process of high-end semiconductor devices, can effectively improve the conductivity and the radiation and interference resistance of the semiconductor devices, and greatly reduces the occurrence of single event effect.
The U.S. has begun research on the separation of boron isotopes as early as the last century and has been successfully industrialized. The research in the field is started late in China, and although a plurality of research results are published, the capability of industrially and stably producing the boron isotope is not available until now.
Chinese patent CN102774845A discloses a method for producing boron trifluoride-11, wherein boron trifluoride feed gas and anisole are complexed in a synthesis device to form a complex, the complex is conveyed to the top of a chemical exchange tower by a pump, boron trifluoride from a cracking device enters from the bottom of the chemical exchange tower and fully contacts through gas-liquid countercurrent at 15-30 ℃, heavier boron-11 isotopes are enriched at the top of the tower in a gas form, lighter boron-10 isotopes are enriched in a liquid phase complex at the bottom of the tower, and finally the abundance of boron-11 in boron trifluoride gas can reach more than 99.7%.
Chinese patent CN102115093B discloses a preparation method of high-purity enriched boron-11 boron trifluoride gas, which adopts a double-tower series process to improve the abundance of boron-11, firstly, boron trifluoride-methyl ether complex is added at one time, then, intermittent rectification is carried out under the negative pressure condition, so that boron-11 is enriched in reflux liquid at the top of a first-stage tower, boron-10 is enriched in a second-stage tower kettle, and finally, the boron trifluoride-methyl ether complex with the abundance of 95% and the purity higher than 99% is obtained at the top of the first-stage tower.
Chinese patent CN108275691B discloses a method and a system for simultaneously producing highly concentrated boron-10 and boron-11 boron trifluoride, wherein the extraction section adopts a multi-tower cascade process to enrich boron-11 isotopes, the gas from the top of the first-stage extraction tower directly flows into the bottom of the next-stage extraction tower through a gas pipeline, the complex compound flowing out from the bottom of the last-stage extraction tower is sent to the top of the previous-stage extraction tower through a liquid pipeline and a metering pump, in each stage of extraction tower, gas-liquid two-phase countercurrent contact is carried out for isotope exchange, and finally, a highly concentrated boron-11 product is obtained at the top of the last-stage extraction tower, and the abundance can reach more than 99%.
In the above patent, CN102774845A adopts the most basic chemical exchange process, and single tower is used for isotope enrichment, the process lags behind, the abundance reaches 99.7% and needs hundreds of theoretical plates, the device needs several tens of meters or even hundreds of meters in height, and the industrial scale-up production is difficult. CN102115093B adopts a batch rectification double-tower series process, the abundance of boron-11 in the first tower is improved, then the boron-11 enters the second tower to improve the abundance continuously, although the total height of the device is reduced, each tower is provided with a condenser and a reboiler, and the energy consumption is increased. Meanwhile, the batch process is not favorable for industrial scale-up production. CN108275691B adopts the multiple-tower cascade technology to enrich boron-11 continuously, and the towers are connected through gas phase pipelines and liquid phase pipelines, and liquid is conveyed by using a pump, although the energy consumption is greatly reduced, in order to achieve higher abundance, three or more stages of extraction tower cascade are needed, the equipment is more, the occupied area is large, and the industrial production is not facilitated.
Meanwhile, CN102115093B and CN108275691B adopt a multi-tower process to enrich boron-11, both use pipelines as connecting channels between towers, and CN108275691B also uses pumps to convey liquid complexes between towers, which undoubtedly increases the complexity of the process, increases the control difficulty, reduces the whole operability and stability of the device, and is very unfavorable for the stable production of boron isotopes.
Disclosure of Invention
The invention aims to provide a production method of a high-abundance boron-11 isotope, which simplifies the prior complex processes of series connection and cascade connection, greatly improves the production stability, improves the enrichment efficiency of boron-11, reduces the energy consumption and the like. In addition, the boron-11 isotope produced by the method has an abundance of 99.9% or more.
The purpose of the invention can be realized by the following technical scheme:
a method for producing abundant boron-11 isotope is characterized in that boron trifluoride is continuously fed from the bottom of a gas-liquid exchange device, complexing agents capable of complexing and reacting with boron trifluoride raw materials continuously enter from the top and the middle of the gas-liquid exchange device, the boron trifluoride and the complexing agents are in countercurrent contact in the gas-liquid exchange device, and products rich in boron-11 are continuously extracted from a top outlet and/or a middle outlet of the gas-liquid exchange device.
Further, the complexing agent is a substance which can react with boron trifluoride to generate a boron trifluoride complex, and the substance includes but is not limited to one or a mixture of inorganic oxides, ethers, alcohols, hydrocarbons, halogenated hydrocarbons, organic amines and the like.
Furthermore, the complexing agent is one or a mixture of more of alkyl ether, thioether, aromatic ether, acetonitrile, small molecular alcohol (C4 and below), sulfur dioxide, small molecular hydrocarbon (C4 and below), chloralkane and the like.
Further, the gas-liquid exchange device is a device capable of supplying gas-liquid two-phase countercurrent contact.
Furthermore, the gas-liquid exchange device is a packed tower or a plate tower.
Further, the product rich in boron-11 is boron trifluoride rich in boron-11 and a boron trifluoride complex rich in boron trifluoride-11, and either one or both of the boron trifluoride rich in boron-11 can be produced, but the former is produced at the top of the gas-liquid exchange device, and the latter is produced at the middle of the gas-liquid exchange device.
Further, the amount of the complexing agent entering the gas-liquid exchange device is reduced from bottom to top in sequence.
Further, the amount of the complexing agent required for completely complexing boron trifluoride passing through the cross section of the gas-liquid exchange device is defined as the theoretical amount of the complexing agent, and the actual entering amount of the complexing agent at a certain middle position of the gas-liquid exchange device is smaller than the theoretical amount of the complexing agent at the position.
Furthermore, the molar ratio of the amount of the complexing agent actually entering a certain middle position of the gas-liquid exchange device to the theoretical amount of the complexing agent at the position is 0.3-0.999.
Further, the top pressure of the gas-liquid exchange device is 20 kPa-200 kPa, and the ambient temperature of the gas-liquid exchange device is constant at-80-30 ℃.
Further, the inner diameter of the gas-liquid exchange device is designed to be gradually reduced from bottom to top.
Compared with the prior art, the invention has the following advantages:
(1) the boron-11 isotope product with the abundance of more than 99.9 percent can be obtained by the method
(2) The traditional cascade process tower and the pipeline and the pump required for connection between the towers are not needed, the process is greatly simplified, and the stability is improved
(3) The method has high enrichment efficiency, low energy consumption and small occupied area, and is suitable for industrial production
Drawings
FIG. 1 is a schematic process diagram of an embodiment of the present invention with only overhead take-off;
the notation in the figure is:
1 is a complexing agent inlet, 2 is a boron trifluoride raw material inlet, 3-a bottom outlet, and 4 is a boron-11 product outlet.
Detailed Description
The present invention is further described in the following description of the specific embodiments, which is not intended to limit the invention, but various modifications and improvements can be made by those skilled in the art according to the basic idea of the invention, within the scope of the invention, as long as they do not depart from the basic idea of the invention.
In order to simplify the complex processes of series connection and cascade connection in the past, improve the production stability, simultaneously improve the enrichment efficiency of boron-11, reduce the energy consumption and the like, the invention provides a production method of a high-abundance boron-11 isotope, wherein boron trifluoride is continuously fed from the bottom of a gas-liquid exchange device, complexing agent capable of carrying out complex reaction with boron trifluoride raw material continuously enters from the top and the middle of the gas-liquid exchange device, the boron trifluoride and the complexing agent are in countercurrent contact in the gas-liquid exchange device, and a product rich in boron-11 is continuously extracted from a top outlet and/or a middle outlet of the gas-liquid exchange device.
In some embodiments, the complexing agent is a substance that can react with boron trifluoride to form a boron trifluoride complex, and includes, but is not limited to, one or a mixture of several of inorganic oxides, ethers, alcohols, hydrocarbons, halogenated hydrocarbons, organic amines, and the like, and specifically may be one or a mixture of several of alkyl ethers, thioethers, aromatic ethers, acetonitrile, small molecular alcohols (C4 and below), sulfur dioxide, small molecular hydrocarbons (C4 and below), chloroalkanes, and the like.
In some embodiments, the gas-liquid exchange device is a device capable of providing gas-liquid two-phase countercurrent contact, and specifically, the gas-liquid exchange device may be a packed column or a plate column, and the like.
In some embodiments, the boron-11 enriched product is boron trifluoride enriched in boron-11 and boron trifluoride complex enriched in boron-11, and specifically, boron trifluoride enriched in boron-11 can be continuously withdrawn from the top outlet of the gas-liquid exchange device, while boron trifluoride complex enriched in boron-11 can be continuously withdrawn from the middle outlet of the gas-liquid exchange device.
In some embodiments, the amount of complexing agent entering the gas-liquid exchange device decreases sequentially from bottom to top.
In some embodiments, the amount of complexing agent required to completely complex boron trifluoride passing through the cross-section of the gas-liquid exchange device is defined as the theoretical amount of complexing agent, and the actual amount of complexing agent entering at a central location in the gas-liquid exchange device is less than the theoretical amount of complexing agent at that location.
Furthermore, the molar ratio of the amount of the complexing agent actually entering a certain middle position of the gas-liquid exchange device to the theoretical amount of the complexing agent at the position is 0.3-0.999, preferably 0.5-0.992, more preferably 0.8-0.99, preferably 0.9-0.98, and most preferably 0.94-0.97.
In some embodiments, the top pressure of the gas-liquid exchange device is 20kPa to 200kPa, and the gas-liquid exchange device is kept at a constant temperature of-80 to 30 ℃, preferably-60 to 25 ℃, more preferably-30 to 20 ℃, preferably 0 to 15 ℃.
In some embodiments, the inner diameter of the gas-liquid exchange device is designed to be gradually reduced from bottom to top, so that the pressure drop per unit height in the gas-liquid exchange device is basically the same, the gas-liquid exchange in all positions is in a reasonable range, and the efficiency of the device is maximized. Certainly, from the practical operation angle, the inner diameter of the gas-liquid exchange device can be changed by adopting a sectional type, namely, the gas-liquid exchange device is formed by combining a plurality of sections with gradually reduced inner diameters from bottom to top.
In some embodiments, the pressure drop per unit height in the gas-liquid exchange device is from 50Pa to 1000Pa, preferably from 100Pa to 800Pa, more preferably from 200Pa to 600Pa, and most preferably from 300Pa to 500 Pa.
In some embodiments, the complex extracted from the bottom of the gas-liquid exchange device is pyrolyzed to obtain boron trifluoride and the complexing agent again, and the complexing agent can be recycled after impurity removal by rectification and water removal by adsorption.
In some embodiments, flow control devices are used to stably control the flow of various streams to and from the gas-liquid exchange device.
The method for producing boron-11 isotopes used in the present invention essentially belongs to the chemical exchange method in the field of isotope separation. It has been found that two molecules contain two stable isotopes of an element at the same time, and that the isotopic ratio of the element in each molecule changes after a period of contact. Further studies have shown that isotopes have different tendencies towards different compounds, and that at natural abundance, there is a tendency for certain isotopes to switch from low-tendency molecules to high-tendency molecules. The chemical exchange method is a method for utilizing and amplifying the tendentiousness of the isotope so as to achieve the purpose of isotope separation.
Because the separation of the boron isotope requires a very high theoretical plate, the traditional series connection and cascade connection process separates the whole equipment into a plurality of sections which are horizontally arranged and are connected with each other through a pipeline and a pump, thereby reducing the whole height of the device and reducing the implementation difficulty. The invention uses the process design that the complexing agent enters from top to bottom in a segmented way, simplifies the traditional complex processes of series connection and cascade connection, reduces the pipelines and pumps between the connecting towers which are indispensable in the series connection and cascade connection processes, and improves the stability of the system.
In addition, the efficiency of gas-liquid mass transfer devices tends to decrease as the diameter becomes larger, as is well known in the art. In particular, when the diameter is below 80mm, the efficiency of the gas-liquid mass transfer device may be much greater than that of, for example, a gas-liquid mass transfer device having a diameter above 150 mm. However, smaller diameters represent lower capacities and industrial production requires finding a balance between the two, and generally, the industry rarely uses devices with diameters below 80 mm. The invention adopts a method of sectionally entering complexing agent, so that the molar flow of gas and liquid phases in the device is changed, the inner diameter of the device can be gradually reduced from bottom to top during implementation, and the unit separation efficiency is gradually improved from bottom to top. Compared with the traditional process, the overall efficiency is improved by 50-100%.
In the present invention, the temperature of the gas-liquid exchange device and the stable control thereof are important. The complexation reaction of boron trifluoride and complexing agent is exothermic, and the reaction temperature will directly affect the degree of complexation reaction. In particular, the influence of the excessive temperature on the complexation reaction is particularly remarkable. For example, it was found through continuous experiments that the degree of complexation between anisole and boron trifluoride reached essentially the theoretical value at 20 ℃ but only 95% of the theoretical value at 30 ℃, which had a great effect on the boron-11 enrichment efficiency. The optimal temperature ranges corresponding to different complexing agents are different, and the corresponding complexing agents need to be selected during actual production. Temperature fluctuations will lead to variations in the degree of complexation within the apparatus, further affecting the efficiency of enrichment. In stable production, temperature fluctuations will eventually lead to a decrease in boron-11 abundance in the product. For example, it was found through experiments that when anisole was used as a complexing agent, the apparatus temperature was maintained at 20 ℃ and then increased to 30 ℃ within 1 hour, and the abundance of boron-11 immediately decreased by 12%. In actual operation, the gas-liquid exchange device should be controlled within a proper temperature range, and the temperature should be kept stable.
The above embodiments may be implemented individually, or in any combination of two or more.
The above embodiments will be described in more detail with reference to the accompanying drawings and specific examples.
Example 1
The complexing agent adopts anisole and enters from a complexing agent inlet 1 (comprising a top inlet and three middle inlets) of the gas-liquid exchange device, and boron trifluoride enters from a boron trifluoride raw material inlet 2 (namely a bottom inlet) of the gas-liquid exchange device. Boron trifluoride-anisole complex is withdrawn from the bottom outlet 3 of the gas-liquid exchange apparatus, and boron trifluoride enriched with boron-11 is withdrawn from the boron-11 product outlet 4 of the gas-liquid exchange apparatus (i.e., the top outlet thereof).
The flow rate change of boron trifluoride in the gas-liquid exchanger and the positions of the inlet and outlet of the material flow are shown in FIG. 1, and the molar flow rate of boron trifluoride in the gas-liquid exchanger gradually decreases from bottom to top, while the flow rate of anisole gradually increases. The molar flow of the boron trifluoride raw material is 5kmol/h, and the entering molar flow of the anisole from bottom to top is 4kmol/h, 0.9kmol/h, 0.09kmol/h and 0.0095kmol/h in sequence. In the whole gas-liquid exchange device, the molar flow rates of boron trifluoride from the bottom of the device to the lower part of a first complexing agent inlet 1 from the bottom of the device to the lower part of a second complexing agent inlet 1 from the bottom of the device to the lower part of a third complexing agent inlet 1 from the lower part of the second complexing agent inlet 1 from the lower part of the third complexing agent inlet 1 to the top complexing agent inlet 1 of the device are 5kmol/h, 1kmol/h, 0.1kmol/h and 0.01kmol/h in sequence. The molar flow rate of boron trifluoride between the lower part of each complexing agent inlet 1 and the complexing agent inlet 1 is rapidly reduced, taking the bottom of the device to the first complexing agent inlet 1 as an example, the molar flow rate of boron trifluoride is kept from bottom to top at 5kmol/h, and the molar flow rate is rapidly reduced to the lower part of the first inlet 1 until the molar flow rate is reduced to 1kmol/h at the first complexing agent inlet 1. The boron-11 enriched boron trifluoride product was withdrawn at a molar flow rate of 0.0005kmol/h and the complex (i.e., boron trifluoride-anisole complex) was withdrawn at a molar flow rate of 4.9995 kmol/h.
The inner diameter of the gas-liquid exchange device is gradually reduced from bottom to top and is divided into four sections, wherein the four sections are 300mm, 125mm, 50mm and 25mm in sequence, and the four sections are 5 meters, 4 meters, 8 meters and 10 meters in sequence. The device is kept at a constant temperature of 20-25 ℃, the temperature at different heights is different, but the temperature at the same height is kept stable. The vapor pressure at the bottom-up anisole entry position was 105.5kPa, 104.5kPa, 103kPa, and 101.5kPa in this order, and the bottom pressure of the apparatus was 106 kPa. The pressure drop per unit height was 100 Pa.
Through detection, the abundance ratio of boron-11 in the boron trifluoride product rich in boron-11 extracted from the top outlet of the gas-liquid exchange device is 99.91%.
Example 2
Dimethyl ether is used as a complexing agent, and enters from a complexing agent inlet 1 (comprising a top inlet and two middle inlets) of the gas-liquid exchange device, and boron trifluoride enters from a boron trifluoride raw material inlet 2 (namely a bottom inlet) of the gas-liquid exchange device. Boron trifluoride-methyl ether complex is extracted from a bottom outlet 3 of the gas-liquid exchange device, boron trifluoride-methyl ether complex rich in boron-11 is extracted from a boron-11 product outlet 4 (here, a middle outlet) of the gas-liquid exchange device, and the middle outlet is positioned between a top complexing agent inlet 1 and a first middle complexing agent inlet 1 from top to bottom.
The molar flow of boron trifluoride in the gas-liquid exchange device is gradually reduced from bottom to top, and the flow of dimethyl ether is gradually increased. The molar flow rate of the boron trifluoride raw material is 5kmol/h, and the entering molar flow rates of dimethyl ether from bottom to top are 4.975kmol/h, 0.02475kmol/h and 0.00025kmol/h in sequence. In the whole gas-liquid exchange device, the molar flow rates of boron trifluoride from the bottom of the device to the lower part of a first complexing agent inlet 1, from the lower part of the first complexing agent inlet 1 to the lower part of a second complexing agent inlet 1, from the lower part of the second complexing agent inlet 1 to the top complexing agent inlet 1 are 5kmol/h, 0.025kmol/h and 0.00025kmol/h in sequence. The molar flow rate of boron trifluoride between the lower part of each complexing agent inlet 1 and the complexing agent inlet 1 is rapidly reduced, taking the bottom of the device to the first complexing agent inlet 1 as an example, the molar flow rate of boron trifluoride is kept from bottom to top at 5kmol/h, and the molar flow rate is rapidly reduced to the lower part of the first inlet 1 until the molar flow rate is reduced to 0.025kmol/h at the first complexing agent inlet 1. The boron-11-rich boron trifluoride-methyl ether complex product was withdrawn at a molar flow rate of 0.00025kmol/h and the complex (i.e., boron trifluoride-methyl ether complex) was withdrawn at a molar flow rate of 4.99975 kmol/h.
The inner diameter of the gas-liquid exchange device is gradually reduced from bottom to top and is divided into three sections, wherein the three sections are 300mm, 45mm and 20mm in sequence, and the heights of the three sections are 6 meters, 10 meters and 14 meters in sequence. The device is kept at a constant temperature of-65 to-60 ℃, the temperature at different heights is different, but the temperature at the same height is kept stable. The vapor pressure from the bottom to the top of the entry point of dimethyl ether was 30kPa, 28kPa, and 26kPa in this order, and the bottom pressure of the apparatus was 33 kPa. The pressure drop per unit height was 80 Pa.
Through detection, the abundance of boron-11 in the boron trifluoride-methyl ether complex product rich in boron-11 and collected from the middle outlet of the gas-liquid exchange device is 99.90%.
Comparative example 1
The conventional constant diameter single column process was used with a constant apparatus internal diameter of 300mm and the same height as in example 1. The anisole enters only from the top, and the molar flow of boron trifluoride in the apparatus from bottom to top is unchanged. The inlet molar flow rate of anisole is 4.9995kmol/h, the molar flow rate of boron trifluoride raw material is 5kmol/h, the extraction molar flow rate of boron trifluoride product rich in boron-11 is 0.0005kmol/h, and the extraction molar flow rate of complex is 4.9995 kmol/h. The bottom pressure of the apparatus was 106kPa, and the top pressure was 101.5 kPa. The rest is the same as example 1.
Through detection, the abundance ratio of boron-11 in the boron trifluoride product rich in boron-11 extracted from the top of the gas-liquid exchange device is 94.88%.
Comparative example 2
A three-tower cascade flow is adopted, the inner diameters of the three devices are all 300mm, and the heights of the three devices are the same as those in the embodiment 1. Anisole enters from the top of the first stage device, is extracted from the bottom of the first stage device and enters the top of the next stage through a pump, boron trifluoride raw material enters from the bottom of the third stage device, is extracted from the top of the third stage device and enters the bottom of the previous stage, finally, a complex compound is extracted from the bottom of the third stage device, and boron trifluoride gas rich in boron-11 is extracted from the top of the first stage device. The inlet molar flow rate of anisole is 4.9995kmol/h, the molar flow rate of boron trifluoride raw material is 5kmol/h, the extraction molar flow rate of boron trifluoride product rich in boron-11 is 0.0005kmol/h, and the extraction molar flow rate of complex is 4.9995 kmol/h. The top pressures of the first, second and third stage units were 102kPa, 105kPa and 108kPa, respectively. The temperature in the device is controlled to be 20-25 ℃, the temperature at different heights is different, but the temperature at the same height is the same and is kept stable.
Through detection, the abundance of boron-11 in the boron trifluoride product rich in boron-11 extracted from the top of the gas-liquid exchange device is 99.90%.
Comparative example 3
The device is kept at a constant temperature of 30-35 ℃, the temperature at different heights is different, but the temperature at the same height is kept stable, and the rest is the same as that in the embodiment 1.
Through detection, the abundance of boron-11 in the boron trifluoride-methyl ether complex product rich in boron-11 and collected from the middle outlet of the gas-liquid exchange device is 96.15%.
Example 1 compares to comparative example 1, which shows that the boron isotopic enrichment efficiency is low using the conventional chemical exchange method, and the abundance of boron-11 enriched at the top is less than 95% at the same operating flow rate and the same height of the device. Compared with the comparative example 2, the embodiment 1 shows that at least three devices with the same height can achieve the enrichment effect in the embodiment 1 by adopting the cascade process, and the device is relatively large in occupied area and complex. Example 1 compares with comparative example 3 to show that temperature control in the apparatus directly affects the gas-liquid exchange effect and that temperature is not suitable to reduce the abundance of boron-11 in the product.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A production method of a high-abundance boron-11 isotope is characterized in that boron trifluoride is continuously fed from the bottom of a gas-liquid exchange device, complexing agents capable of carrying out complexing reaction with a boron trifluoride raw material continuously enter from the top and the middle of the gas-liquid exchange device, the boron trifluoride and the complexing agents are in countercurrent contact in the gas-liquid exchange device, and a product rich in boron-11 is continuously extracted from a top outlet and/or a middle outlet of the gas-liquid exchange device.
2. The method for producing a high abundance boron-11 isotope according to claim 1, wherein the complexing agent is a substance that can react with boron trifluoride to form a boron trifluoride complex, and the substance includes one or more of inorganic oxides, ethers, alcohols, hydrocarbons, halogenated hydrocarbons, and organic amines.
3. The method for producing a high abundance boron-11 isotope according to claim 1, wherein the gas-liquid exchange device is a device capable of gas-liquid two-phase countercurrent contact.
4. The method for producing a high abundance boron-11 isotope according to claim 3, wherein the gas-liquid exchange device is a packed column or a plate column.
5. The method for producing a high abundance boron-11 isotope according to claim 1, wherein the boron-11 rich product is boron trifluoride rich in boron-11 and a boron trifluoride complex rich in boron-11.
6. The method for producing a high abundance boron-11 isotope according to claim 1, wherein the amount of the complexing agent introduced into the gas-liquid exchange device decreases from bottom to top.
7. The method for producing an abundant boron-11 isotope according to claim 1, wherein the amount of the complexing agent required for completely complexing boron trifluoride passing through the cross section of the gas-liquid exchange apparatus is defined as a theoretical amount of the complexing agent, and an actual amount of the complexing agent entering a position in a middle of the gas-liquid exchange apparatus is smaller than the theoretical amount of the complexing agent at the position.
8. The method for producing a high abundance boron-11 isotope according to claim 7, wherein the molar ratio of the amount of complexing agent actually introduced to a central position of the gas-liquid exchange device to the theoretical amount of complexing agent at that position is 0.3 to 0.999.
9. The method for producing the abundant boron-11 isotope according to claim 1, wherein the top pressure of the gas-liquid exchange device is 20kPa to 200kPa, and the ambient temperature of the gas-liquid exchange device is constant at-80 ℃ to 30 ℃.
10. The method for producing the abundant boron-11 isotope according to claim 1, wherein the inner diameter of the gas-liquid exchange device is designed to be gradually reduced from bottom to top.
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| CN115608156A (en) * | 2022-12-19 | 2023-01-17 | 淄博颐康环保科技有限公司 | Sectional type cooling complexing device and complexing method for separating boron isotopes |
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| CN112279261A (en) * | 2020-11-03 | 2021-01-29 | 山东合益气体股份有限公司 | Preparation method of neutron lens grade boron 11 |
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| CN115608156A (en) * | 2022-12-19 | 2023-01-17 | 淄博颐康环保科技有限公司 | Sectional type cooling complexing device and complexing method for separating boron isotopes |
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