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Ion hybridization porous material and preparation method and applications thereof

A porous material and hybridization technology, applied in separation methods, chemical instruments and methods, organic chemistry, etc., can solve the problems of difficult design and preparation, achieve remarkable removal effect, simple preparation method, and good acetylene capture capacity Effect

Active Publication Date: 2019-03-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The pore structure, active sites and separation properties of ion hybrid porous materials are closely related to the types of organic ligands and metal ions. Designing new structure ion hybrid materials is crucial for their applications, but the design and preparation are difficult

Method used

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  • Ion hybridization porous material and preparation method and applications thereof
  • Ion hybridization porous material and preparation method and applications thereof
  • Ion hybridization porous material and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 1mmol 4,4’-bipyridine disulfide in 20ml methanol solution dropwise to 0.5 mmol(NH 4 ) 2 GeF 6 And 0.5mmol Cu(BF 4 ) 2 In 10ml aqueous solution, magnetically stirred at room temperature for 24h, and after suction filtration, the product was soaked in methanol for 24h to obtain GeFSIX-S-Cu-i ion hybrid porous material.

[0039] The adsorption isotherm of GeFSIX-S-Cu-i for acetylene and ethylene at 298K is as figure 1 As shown; the XRD data graph is as figure 2 Shown.

[0040] Load the obtained GeFSIX-S-Cu-i ion hybrid porous material into a 5cm long adsorption column, and pass the ethylene:acetylene (volume ratio 99:1) mixed gas 1.0ml / min into the adsorption column of the embodiment at 25°C , To obtain high-purity ethylene gas (greater than 99.999%), when the acetylene penetrates, stop the adsorption, and purge the adsorption column with He gas for 18h, the adsorption column can be recycled.

Embodiment 2

[0042] Add 0.85mmol of 4,4'-bipyridine disulfide in ethanol and ethylene glycol (1:1) solution dropwise to 0.3mmol of NiTiF 6 The reaction was carried out at 65°C for 12h in the aqueous solution, and the product obtained was filtered and washed with suction to obtain TIFSIX-S-Ni-i ion hybrid porous material.

[0043] The crystal structure diagram of TIFSIX-S-Ni-i is as follows image 3 As shown; the XRD data graph is as Figure 4 Shown.

Embodiment 3

[0045] Add 1mmol 4,4’-bipyridinedisulfide in 20ml methanol solution dropwise to 0.5mmol CuZrF 6 In 20ml methanol solution, magnetically stirred at room temperature for 24h, and after suction filtration, the product obtained was soaked in methanol for 24h to obtain the ZrFSIX-S-Cu-i ion hybrid porous material.

[0046] The adsorption and desorption isotherm of acetylene by ZrFSIX-S-Cu-i at 273K is as Figure 5 Shown.

[0047] Load the obtained ZrFSIX-S-Cu-i ion hybrid porous material into a 10cm long adsorption column, and pass 1.0ml / min of ethylene:acetylene (volume ratio 50:50) mixed gas into the adsorption column of the embodiment at 25°C , To obtain high-purity ethylene gas (greater than 99.99%), when the acetylene penetrates, stop the adsorption. The adsorption column adopts vacuum desorption to obtain acetylene gas with a purity greater than 90%, and the adsorption column can be recycled.

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Abstract

The invention discloses an ion hybridization porous material and a preparation method and applications thereof. The ion hybridization porous material is constructing by connecting a disulfide organicligand, an inorganic fluorine containing anion, and a metal ion through coordination bonds. The expression formula of the porous material is M-L-AO<x>F<6-x>; wherein the metal ion M is any one of Fe<2+>, Co <2+>, Ni<2+>, Cu<2+>, and Zn<2+>; and the inorganic fluorine containing anion AO<x>F<6-x> is any one of SiF6<2->, ZrF6<2->, SnF6<2->, TiF6<2->, WO2F4<2->, and MoO2F4<2->. The ion hybridizationporous material is prepared by an interface diffusion method, a room temperature stirring method or a solvothermal method; and is applied to acetylene / ethylene adsorption separation or allylene / allene / propylene adsorption separation.

Description

Technical field [0001] The invention belongs to the technical field of new chemical materials, and specifically relates to an ion hybrid porous material, a preparation method and an application. Background technique [0002] Ion hybrid porous materials have attracted more and more attention because of their variable structure and adjustable pore structure, and their excellent performance in the fields of gas adsorption and separation. Such materials usually use metal ions or ion clusters as contact points, and use organic ligands and inorganic anions as pillared bodies to construct a three-dimensional structure with regular internal arrangement. Compared with traditional porous materials such as molecular sieves, this material not only has the characteristic of unlimited extension of crystals, but also has metal-heteroatom bonds. Based on the above characteristics, the ion hybrid porous material has a larger specific surface area and a higher pore volume, which makes it have a g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D53/02C07D311/72C07J9/00
CPCB01D53/02B01J20/223C07D311/72C07J9/00
Inventor 邢华斌张照强杨启炜任其龙杨亦文
Owner ZHEJIANG UNIV
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