Layered fluorine-containing metal-organic framework material for adsorbing and separating ethynyl ethylene and preparation method and application thereof
An organic framework, adsorption separation technology, applied in the direction of adsorption purification/separation, organic chemistry, alkali metal compounds, etc., can solve the problems of harsh adsorption conditions and limit the application of adsorption separation, and achieve simple preparation method, significant removal effect, excellent Effect of Acetylene/Ethylene Selective Separation Properties
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Embodiment 1
[0076] Adopt room temperature stirring synthesis method, 0.5mmol Cu(BF 4 ) 2 and 0.5mmol (NH 4 ) 2 TiF 6 Dissolve in deionized water, dissolve 1mmol 4,4'-dipyridine sulfone in anhydrous methanol, mix the two, react at 25°C for 24h to obtain crystals, filter the obtained crystals, wash with methanol, and dry to obtain Cu(4,4' -dipyridylsulfone) 2 TiF 6 .
[0077] 1. Cu(4,4'-dipyridylsulfone) 2 TiF 6 Structure
[0078] Cu(4,4'-dipyridylsulfone) 2 TiF 6 It is a metal-organic framework material with a layered three-dimensional structure. Crystal structure such as figure 1 As shown, the metal copper ion forms a pseudo one-dimensional chain structure (ab plane) with the organic ligand 4,4’-dipyridine sulfone, and then interacts with the inorganic fluorine-containing anion TiF 6 2- A two-dimensional network with one-dimensional channels is formed by bridging in the c-axis direction, and a layered three-dimensional structure with permanent three-dimensional through chann...
Embodiment 2
[0084] Penetration testing of gas mixtures
[0085] With embodiment 1 gained Cu (4,4'-dipyridylsulfone) 2 TiF 6 The material was packed into a 5 cm long adsorption column (inner diameter 4.6 mm), and the sample was first purged with He flow (15 mL / min) at 65 °C for 24 hours. Then, at 25 °C, 1 bar of acetylene: ethylene (volume ratio 1:99) gas mixture was passed through the adsorption column at 1.25 mL / min, and gas chromatography (GC2010Pro, SHIMADZU) with a flame ionization detector (FID) was used to monitor the gas from the tube. Exhaust gas from the column outlet. High-purity ethylene (greater than 99.9999%) gas can be obtained in the effluent gas. Breakthrough curves such as Figure 4 shown. After testing, ethylene breaks through in 48 minutes, acetylene starts to break through in 2200 minutes, and the dynamic adsorption capacity of acetylene is 1.9mmol / g. The two gases are effectively separated. After 5 adsorption-regeneration cycles, the adsorption performance of t...
Embodiment 3
[0087] Penetration testing of gas mixtures
[0088] With embodiment 1 gained Cu (4,4'-dipyridylsulfone) 2 TiF 6 The material was packed into a 5 cm long adsorption column (inner diameter 4.6 mm), and the sample was first purged with He flow (15 mL / min) at 65 °C for 24 hours. Then, at 25°C, 1 bar of acetylene: ethylene (volume ratio 10:90) gas mixture was introduced into the adsorption column at 1 mL / min, and gas chromatography (GC2010Pro, SHIMADZU) with a flame ionization detector (FID) was used to monitor Export exhaust. High-purity ethylene (greater than 99.9999%) gas can be obtained in the effluent gas. The adsorption column can be recycled after regeneration.
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