A kind of xenon gas krypton separation method

A separation method, xenon technology, applied in chemical instruments and methods, inert gas compounds, other chemical processes, etc., can solve the problem of high adsorption capacity and high selectivity, low adsorption capacity and selectivity, affecting industrial application value. and other problems, to achieve the effect of high selectivity, high adsorption and separation selectivity, and low equipment investment

Active Publication Date: 2020-12-15
ZHEJIANG UNIV
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Problems solved by technology

The key to this technology is to develop adsorbent materials with both high capacity and high selectivity. However, the existing adsorbent materials often have the phenomenon that high adsorption capacity and high selectivity cannot be achieved at the same time, which seriously affects their industrial application value.
[0005] For example, the traditional solid adsorbent NaA molecular sieve has an adsorption capacity of 20% to 30% for xenon, and a selectivity of only 4 to 6 (100kPa, 298K). The lower adsorption capacity and selectivity limit their application (J .Chem.Phys,1997,107(11):4364-4372)
As another example, CC3, a porous organic molecular cage, is used for the separation of xenon and krypton. The adsorption capacity of CC3 to xenon and krypton is 2.42 and 0.92 mmol / g (100kPa, 298K) respectively, and the ratio of adsorption capacity is only 2.63. Low separation selectivity (Nature Materials,2014,13(10):954-960)
In addition, the metal-organic framework material SBMOF-2 shows a strong adsorption force for xenon, which increases the adsorption capacity of xenon to 2.83mmol / g (100kPa, 298K), but because it still has a certain amount of adsorption for krypton ( 0.9mmol / g), which limits its separation selectivity (Journal of the American Chemical Society, 2015,137(22):7007-7010)
[0006] Therefore, it is still a big challenge to develop adsorbent materials with both high capacity and high selectivity to realize the efficient separation of xenon and krypton.

Method used

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  • A kind of xenon gas krypton separation method
  • A kind of xenon gas krypton separation method
  • A kind of xenon gas krypton separation method

Examples

Experimental program
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Effect test

Embodiment 1

[0048] 1mmol Cu(BF 4 ) 2 , 1mmol KNbF 6 Dissolve 1.5mmol of 1,2-dipyridylacetylene in 10mL of methanol in 10mL of water, mix the two and stir at room temperature for 24h, and then activate the slurry at room temperature for 24h under vacuum after suction filtration to obtain NbFSIX-2-Cu -i material.

[0049] The single-component adsorption isotherms of xenon and krypton were measured for NbFSIX-2-Cu-i material at 273K and 298K, and the results are as follows: figure 2 , 3 shown.

[0050] The obtained NbFSIX-2-Cu-i material was filled into a 5cm adsorption column, and a 0.1MPa xenon / krypton (molar ratio 20:80) gas mixture was passed into the adsorption column at 0°C at 3.5mL / min, and the gas flowed out High-purity krypton gas (greater than 99.9%) gas can be obtained in the medium, and when xenon gas penetrates, the adsorption stops. Afterwards, nitrogen gas is switched to purge the adsorption column at room temperature, and the flow rate is 3.0 mL / min to obtain high-puri...

Embodiment 2

[0054] 1mmol ZnZrF 6 Dissolve 1.5mmol of 1,2-dipyridineacetylene in 10mL of methanol, mix the two at room temperature and stir for 24h, and then activate the slurry at room temperature for 24h under vacuum after suction filtration to obtain ZrFSIX-2-Zn -i material.

[0055] The single-component adsorption isotherm of xenon and krypton was measured for ZrFSIX-2-Zn-i material at 273K, and the results are as follows Image 6 shown.

[0056] The obtained ZrFSIX-2-Zn-i material was filled into a 5cm adsorption column, and a 0.1MPa xenon / krypton (molar ratio 20:80) gas mixture was passed into the adsorption column at 0°C at 3.5mL / min, and the gas flowed out High-purity krypton gas (greater than 99.9%) gas can be obtained in the medium, and when xenon gas penetrates, the adsorption stops. The adsorption column is purged with nitrogen at room temperature to obtain high-purity xenon gas (purity greater than 90%), and the adsorption column can be recycled.

Embodiment 3

[0058] 1mmol CuZrF 6 Dissolve 1.5mmol of 1,2-dipyridineacetylene in 10mL of methanol, mix the two at room temperature and stir for 24h, and then activate the slurry at room temperature for 24h under vacuum after suction filtration to obtain ZrFSIX-2-Cu -i material.

[0059] The single-component adsorption isotherm of xenon and krypton was measured for ZrFSIX-2-Cu-i material at 273K, and the results are as follows Figure 7 shown;

[0060] The obtained ZrFSIX-2-Cu-i material was filled into a 5cm adsorption column, and a 0.1MPa xenon / krypton (molar ratio 20:80) gas mixture was passed into the adsorption column at 0°C at 3.5mL / min, and the gas flowed out High-purity krypton gas (greater than 99.9%) gas can be obtained in the medium, and when xenon gas penetrates, the adsorption stops. The adsorption column is purged with nitrogen at room temperature to obtain high-purity xenon gas (purity greater than 85%), and the adsorption column can be recycled.

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Abstract

The invention discloses a xenon-krypton separation method. A fluorine-containing anion hybridized ultramicropore material with a flexible function is adopted to selectively adsorb xenon in a mixed xenon-krypton gas, and then separation of xenon from krypton is achieved; and the fluorine-containing anion hybridized ultramicropore material with the flexible function has a structural formula of M-(C12H8N2)-AF6 or M-(C10H8N2S2)-AF6, in the formula, C12H8N2 is an organic ligand 1,2-bipyridine acetylene, C10H8N2S2 is an organic ligand 4,4'-dipyridinyl disulfide, M is a metal ion, and AF6 is inorganic fluorine-containing anion. Compared with a common adsorbent, the fluorine-containing anion hybridized ultramicropore material with the flexible function, which is disclosed by the invention, has theadvantages of being adjustable in pore structure, adjustable in action with adsorbate molecules, and meanwhile has a high adsorption capacity and high selectivity.

Description

technical field [0001] The invention relates to the technical field of gas separation, in particular to a method for separating xenon and krypton. Background technique [0002] The inert gases xenon and krypton are important industrial gases in the national economy. Due to their special physical properties, they are widely used in the fields of electronics, medicine, electric light source, gas laser, plasma flow and semiconductor. Xenon and krypton mainly come from the air, and the content is extremely low, only 0.087ppmv and 1ppmv. At present, with the economic recovery, the rapid development of new industries will greatly increase the demand for xenon and krypton. [0003] At present, the industry mainly produces high-purity xenon and krypton through low-temperature distillation. In a large-scale air separation unit, a high-concentration mixture of xenon and krypton is separated as a by-product. In order to obtain high-purity xenon and krypton, the mixture needs to be se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B23/00B01J20/22B01J20/28B01J20/30
CPCB01J20/223B01J20/2808B01J20/28097C01B23/0057
Inventor 邢华斌王青菊杨启炜崔希利
Owner ZHEJIANG UNIV
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