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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

Active Publication Date: 2020-06-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

From Figure S16 of this document, it can be seen that the adsorption of acetylene by UTSA-300a at room temperature (298K) requires a certain pressure condition (about 150-200mmHg acetylene pressure). Higher partial pressure of acetylene can achieve the adsorption of acetylene, which limits the application of this material to the adsorption and separation of low content of acetylene (low acetylene partial pressure) in the mixed gas

Method used

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  • Layered fluorine-containing metal-organic framework material for adsorbing and separating ethynyl ethylene and preparation method and application thereof
  • Layered fluorine-containing metal-organic framework material for adsorbing and separating ethynyl ethylene and preparation method and application thereof
  • Layered fluorine-containing metal-organic framework material for adsorbing and separating ethynyl ethylene and preparation method and application thereof

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Experimental program
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Effect test

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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Abstract

The invention discloses a layered fluorine-containing metal-organic framework material for adsorbing and separating acetylene ethylene, the structural general formula is ML2A, M is a metal ion, L is abroken line type organic ligand, A is an inorganic fluorine-containing anion, and the metal ion M is at least one of Cu<2+>, Fe<2+>, Co<2+>, Ni<2+> and Zn<2+>, wherein the broken line type organic ligand L is at least one of 4, 4'-dipyridylsulfoxide and 4, 4'-dipyridylsulfone, and the inorganic fluorine-containing anion A is at least one of SiF6<2->, GeF6<2->, ZrF6<2->, SnF6<2->, TiF6<2->, NbOF52<->, WO2F4<2-> and MoO2F4<2->. The layered fluorine-containing metal-organic framework material can be prepared by adopting an interface diffusion method, a solvothermal method or a room-temperature stirring method. The layered fluorine-containing metal-organic framework material is used as an adsorbent and is in contact adsorption with a gas mixture containing acetylene and ethylene, and efficient separation of acetylene / ethylene can be realized at normal temperature, low acetylene content and low acetylene partial pressure.

Description

technical field [0001] The invention relates to the technical field of chemical separation, in particular to a layered fluorine-containing metal-organic framework material for adsorption and separation of ethylene acetylene and its preparation method and application. Background technique [0002] As one of the chemicals with the largest output in the world, ethylene is widely used in the synthesis of plastics, rubber, polymer intermediates, etc. In 2018, the global ethylene output was about 170 million tons, and its output is an important standard to measure the development level of the country's petrochemical industry One of them is known as the "mother of petrochemical industry". Acetylene is often used in lighting, burning to generate high temperature to cut and weld metal; at the same time, it is used as a basic raw material to prepare acetaldehyde, acetic acid, synthetic fiber, synthetic rubber, etc. Ethylene is mainly separated from petroleum cracking gas. In the proc...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C07C7/12C07C11/04C07C11/24C08G83/00
CPCB01J20/226B01J20/28033B01J20/28035B01J2220/4812C07C7/12C08G83/008C07C11/04C07C11/24
Inventor 杨启炜沈瑾任其龙柯天杨亦文张治国鲍宗必
Owner ZHEJIANG UNIV
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