Metal-organic framework material for separating xenon and krypton and method for separating xenon and krypton

A technology of metal-organic frameworks and metal ions, applied in separation methods, chemical instruments and methods, and separation of dispersed particles, can solve the problems of easy structure collapse, loss of separation performance, poor stability, etc., and achieve stable performance and good adsorption and separation effects , The effect of stable structural performance

Active Publication Date: 2018-11-02
ZHEJIANG UNIV
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Problems solved by technology

Thallapally et al. used metal organic framework material Ni-MOF-74 to effectively realize the separation of xenon and krypton (Facile xenon capture and release at room temperature using metal–organic framework: a comparison with activated charcoal.Chem.Commun.,2012,48,347 -349), its selectivity reaches 7.3, but the stability of the material is poor when exposed to water, and the structure is easy to collapse in the wet environment containing water vapor and lose the separation performance

Method used

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  • Metal-organic framework material for separating xenon and krypton and method for separating xenon and krypton

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Embodiment 1

[0045] Mix 1.93mmol cobalt chloride hexahydrate, 2.88mmol squaraine, 7.72mmol potassium hydroxide, and 7ml deionized water, put them into a 25mL hydrothermal reactor, stir for 30 minutes, and then heat to 220°C for 48 hours. After the reaction is completed, the reactor is cooled, and the solid obtained from the reaction is washed with pure water several times to obtain a purified metal-organic framework material. The purified adsorbent was vacuum degassed at 120 °C for 12 hours to obtain the desolvated adsorbent, followed by gas adsorption.

[0046] In order to test the adsorption-separation performance of the above-synthesized MOFs, single-component adsorption isotherms of xenon and krypton were carried out using the above-mentioned adsorbents. Take 100 mg of adsorbent and set the adsorption temperature to 25 degrees. After testing, at 25°C and 1bar, the adsorption capacity of xenon reaches 20.8cm 3 / cm 3 , the adsorption capacity of krypton gas is only 13.1cm 3 / cm 3 , ...

Embodiment 2

[0050] Mix 1.93mmol nickel chloride hexahydrate, 2.88mmol squaraine, 3.86mmol potassium hydroxide, and 7mL deionized water, put them into a 25mL hydrothermal reactor, stir for 30 minutes, and react at 220°C for 48 hours. After the reaction is completed, it is cooled and washed with pure water several times to obtain a purified metal-organic framework material. The purified adsorbent was vacuum degassed at 120 °C for 12 hours to obtain the desolvated adsorbent, followed by gas adsorption.

[0051] In order to test the adsorption-separation performance of the above-synthesized MOFs, single-component adsorption isotherms of xenon and krypton were carried out using the above-mentioned adsorbents. Take 100 mg of adsorbent and set the adsorption temperature to 25 degrees. After testing, at 25°C and 1bar, the adsorption capacity of xenon reaches 35.9cm 3 / cm 3 , the adsorption capacity of krypton gas is only 32.7cm 3 / cm 3 , and at a low pressure of 10kPa, the adsorption capacit...

Embodiment 3

[0055] Mix 0.151mmol calcium carbonate, 0.151mmol squaraine, and 20mL deionized water, put them into a 25mL hydrothermal reaction kettle, stir for 30 minutes, and react at 120°C for 24 hours. After the reaction is completed, the reactor is cooled, and washed with pure water for several times to obtain a purified metal organic framework material. The purified adsorbent was vacuum degassed at 100 °C for 12 h to obtain the desolvated adsorbent, followed by gas adsorption.

[0056] In order to test the adsorption-separation performance of the above-synthesized MOFs, single-component adsorption isotherms of xenon and krypton were carried out using the above-mentioned adsorbents. Take 100 mg of adsorbent and set the adsorption temperature to 25 degrees. After testing, at 25°C and 1bar, the adsorption capacity of xenon reaches 75.6cm 3 / cm 3 , the adsorption capacity of krypton gas is only 53.3cm 3 / cm 3 , calculated by IAST, when the volume ratio of xenon / krypton is 20:80, the ...

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Abstract

The invention discloses a metal-organic framework material for separating xenon and krypton and a method for separating xenon and krypton. The metal-organic framework material is good in stability andhigh in adsorptive separation selectivity, the preparation method is simple, and the preparation cost is low. The general structural formula of the metal-organic framework material is [M(C4O4(OH)2).3H2O or [M(C4O4)].2.5H2O, wherein M is metal ions, and transition metal ions or alkaline earth metal ions and squaric acid form a 3D network structure through coordinate bonds or intermolecular actingforce. A preparation method comprises the steps as follows: (1) inorganic salt, squaric acid, alkali and deionized water are mixed in proportion, and the obtained mixture is put in a reactor for a hydrothermal reaction after being stirred to be dissolved, wherein the inorganic salt comprises chlorate, nitrate, acetate, carbonate, sulfate or perchlorate of metal ions; (2) after the hydrothermal reaction, a product is washed with deionized water multiple times, vacuum drying is performed, and the metal-organic framework material is obtained. The metal-organic framework material is used as an adsorbent to perform adsorptive separation on mixed gas containing xenon and krypton.

Description

technical field [0001] The invention relates to a metal organic framework material which can be used for the separation of xenon gas and krypton gas and a preparation method thereof, and belongs to the technical field of adsorption separation materials. Background technique [0002] Xenon (Xe) and krypton (Kr) in noble gases (rare gases) are a very important class of gases. In the air, the content of xenon and krypton is extremely low compared with other non-radioactive inert gases, only 0.087ppmv for xenon and 1.14ppmv for krypton. Because of its special physical properties, it is widely used in the fields of semiconductors, electric light sources, medicine, lasers, catalysis, plasma flow, and some basic scientific research. At present, industrially high-purity xenon and krypton are a type of by-products obtained by low-temperature rectification of air. In the large-scale industrial production process, different products are obtained at different temperatures in the recti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J20/22B01D53/02B01J20/30
CPCB01D53/02B01J20/223C08G83/008
Inventor 鲍宗必李良英任其龙张治国杨亦文杨启炜
Owner ZHEJIANG UNIV
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