Hydrothermally stable anionic pillared porous material and preparation method and applications thereof

A technology of porous materials and anion columns, which is applied in the direction of anion exchanger materials, organic chemical methods, chemical instruments and methods, etc., can solve the problems of inability to balance selectivity and capacity, influence, lack of stability of porous materials, etc., and achieve good Molecular recognition ability, controllable pore structure, and wide range of applicable organic ligands

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

AI Technical Summary

Problems solved by technology

For example, M'MOF (Nat.Commun, 2011, 2(1), 1-7) and MOF-74 (Science, 2012, 335, 1606-1610) have shown certain acetylene separation selectivity, but the selectivity Incompatible with capacity
[0005] For example, the patent CN201610330278.4 reports a method for the separation of propyne mixture using an anionic hybrid material, which has a good separation effect, but the porous material used has a lack of stability in water and heat environments, which affects practical application

Method used

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  • Hydrothermally stable anionic pillared porous material and preparation method and applications thereof
  • Hydrothermally stable anionic pillared porous material and preparation method and applications thereof
  • Hydrothermally stable anionic pillared porous material and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Prefabricated CuNbOF 5 : 0.80g CuO (1mmol), 1.32g Nb 2 o 5 (1.2mmol) in a hydrothermal kettle, add 6mL of hydrofluoric acid (48-50%), and place it at 120°C for 24h to obtain inorganic metal CuNbOF 5 .

[0079] 0.0717g CuNbOF 5 Dissolve 1,2-dipyridylacetylene in 4mL ethylene glycol, then mix, stir at room temperature for 24 hours to obtain a gray powder, filter the product, soak in methanol for 24 hours, and dry to obtain ZU-NbOFFIVE-2- Cu-i.

[0080] ZU-NbOFFIVE-2-Cu-i in Example 1 is packed into a 5cm adsorption column, and at room temperature, 0.1 MPa of acetylene vinyl (1:99) mixed gas is passed into the adsorption column at 1.10mL / min, and high Purity propylene (greater than 99.9999%), when propadiene breaks through, stop adsorption, use inert gas to purge, and the adsorption column can be recycled.

[0081] Put ZU-NbOFFIVE-2-Cu-i in Example 1 into a 5cm adsorption column, and pass 0.1 MPa of propylene propargyl propadiene (0.5:0.5:99) gas mixture into the ads...

Embodiment 2

[0091] Prefabricated CuNbOF 5 : 0.80g CuO (1mmol), 1.32g Nb 2 o 5 (1.2mmol) in a hydrothermal kettle, add 6mL of hydrofluoric acid (48-50%), and place it at 120°C for 24h to obtain inorganic metal CuNbOF 5

[0092] 0.0995g CuNbOF 5 Dissolve 4,4'-azopyridine in 4mL ethanol in 4mL of ethylene glycol, then mix and react at 80°C for 24h to obtain a red powder, filter the product, soak in methanol for 72h, and dry to obtain ZU-NbOFFIVE-14 -Cu-i.

[0093] ZU-NbOFFIVE-14-Cu-i in Example 2 is packed into a 5cm adsorption column, and at room temperature, 0.1 MPa of acetylene vinyl (1:99) gas mixture is passed into the adsorption column at 1.10mL / min, and high Purity propylene (greater than 99.9999%), when propadiene breaks through, stop adsorption, use inert gas to purge, and the adsorption column can be recycled.

[0094] Put ZU-NbOFFIVE-14-Cu-i in Example 2 into a 5cm adsorption column, and pass 0.1 MPa of propylene propargyl propadiene (0.5:0.5:99) gas mixture into the adsorpt...

Embodiment 3

[0102] Prefabricated NiNbOF 5 : 0.74g NiO, 1.584g Nb 2 o 5 Put it in a hydrothermal kettle, add 5mL of hydrofluoric acid (48%-50%), put it at 140°C for 24h, and get green crystal NiNbOF 5 .

[0103] 0.0757g NiNbOF 5 Dissolve 0.05148 g of 1,2-dipyridylacetylene in 5 mL of methanol, then add 1,2-dipyridylacetylene methanol solution dropwise to NiNbOF 5 In the solution, react at 50°C for 24h to obtain light blue powder, filter the product and soak in methanol for 24h.

[0104] ZU-NbOFFIVE-2-Ni-i in Example 3 is packed into a 5cm adsorption column, and at room temperature, 0.1 MPa of acetylene vinyl (1:99) mixed gas is passed into the adsorption column at 1.10mL / min, and high Purity propylene (greater than 99.9999%), when propadiene breaks through, stop adsorption, use inert gas to purge, and the adsorption column can be recycled.

[0105] Put ZU-NbOFFIVE-2-Ni-i in Example 3 into a 5cm adsorption column, and pass 0.1 MPa of propargyl propadiene (0.5:0.5:99) gas mixture into ...

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Abstract

The invention discloses a hydrothermally stable anionic pillared porous material and a preparation method and applications thereof. The hydrothermally stable anionic pillared porous material is prepared from metal ions, an inorganic anion NbOF5<2-> and an organic ligand through self-assembly and the components are connected by coordination bonds. The formula of the porous material is ZU-NbOF5-L-M.The preparation method comprises following steps: mixing a metal oxide (MO), Nb2O5 and hydrofluoric acid according to a certain ratio in a hydrothermal reactor to carry out hydrothermal reactions, and then cooling the hydrothermal reactor in a still state to obtain an inorganic metal ligand MNbOF5; and (2) dissolving M-NbOF5 into a solvent (A) to obtain a solution (A), dissolving an organic ligand (L) into a solvent (B) to obtain a solution (B), adding the solution (A) into the solution (B), stirring, carrying out reactions, after reactions, washing the reaction production by a solvent (C), soaking the reaction product in the solvent (C), and drying to obtain ZU-NbOF5-L-M. The provided hydrothermally stable anionic pillared porous material is used to separate C2-C3 hydrocarbon compounds.

Description

technical field [0001] The invention relates to the technical field of separation materials, in particular to a stable anionic pillared hybrid porous material and its application in the separation of C2 and C3. Background technique [0002] Ethylene propylene, as the two most produced basic chemicals in industrial applications, mainly comes from the cracking of petroleum hydrocarbons. However, no matter whether it is ethylene or propylene obtained by cracking, it is inevitable to be mixed with a small amount of alkynes and some other impurities. These trace impurities will affect the further polymerization of olefins, and even cause catalyst poisoning. [0003] Traditional methods for removing trace alkyne impurities in alkenes include liquid-phase catalytic selective hydrogenation, gas-phase catalytic selective hydrogenation and rectification. However, the disadvantages of hydrogenation mainly lie in the uncontrollable degree of hydrogenation, the secondary hydrogenation o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/00B01J20/22B01J20/30C07C7/12C07C11/04C07C11/06C07C11/22C07C11/14
CPCB01J20/223B01J41/09C07B2200/13C07C7/12C07F9/005C07C11/04C07C11/06C07C11/22C07C11/14Y02P30/40
Inventor 邢华斌杨立峰张照强杨启炜杨亦文
Owner ZHEJIANG UNIV
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