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Metal-organic framework MIL-160 film, preparation method and application

A metal-organic framework, porous alumina technology, applied in organic chemistry, chemical instruments and methods, membrane technology, etc., can solve the problems of low paraxylene flux, cracks, pinhole intergranular, etc., and achieve high selective separation performance Effect

Active Publication Date: 2018-11-27
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In fact, previous studies have shown that MFI molecular sieve membranes exhibit excellent p- / o-xylene separation selectivities with separation factors ranging from tens to hundreds, even as high as 10,000, but the flux of p-xylene through MFI membranes is relatively lower
In addition, since the synthesis of MFI membranes usually requires the use of organic structure directing agents (SDA), the removal of organic structure directing agents (SDA) from the membrane pores by high-temperature calcination easily leads to the generation of cracks, pinholes and other intergranular defects.
Therefore, it is still a great challenge to develop new membrane materials that are easily activated for the separation of xylene isomers.

Method used

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  • Metal-organic framework MIL-160 film, preparation method and application
  • Metal-organic framework MIL-160 film, preparation method and application
  • Metal-organic framework MIL-160 film, preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0022] MIL-160 membranes were synthesized as follows

[0023] Step 1. Modification of Porous Alumina Matrix by Dopamine Functionalization

[0024] Dissolve 0.5 g of dopamine hydrochloride in 70 mL of distilled water, stir and mix evenly, then add tris to control the pH of the solution to 8.5. The washed and dried porous alumina matrix was put into the dopamine buffer solution, reacted at room temperature for 24 hours, rinsed with distilled water and ethanol, and dried at room temperature for 24 hours before use.

[0025] Step 2: MIL-160 film preparation

[0026] Dissolve 0.2g of aluminum trichloride hexahydrate, 0.13g of 2,5-furandicarboxylic acid, and 0.12g of sodium formate in 15g of distilled water, stir magnetically until the solution is clear, and then stir overnight to prepare MIL-160 membrane synthesis solution; Pour the synthesis solution into the reaction kettle with the dopamine-modified porous alumina substrate in step 1. After the reaction kettle was sealed, it ...

Embodiment 2

[0028] MIL-160 films were synthesized as follows:

[0029] Step 1: Modification of Porous Alumina Matrix by Dopamine Functionalization

[0030] Dissolve 0.5 g of dopamine hydrochloride in 70 mL of distilled water, stir and mix evenly, then add tris to control the pH of the solution to 9. Put the washed and dried porous alumina matrix into the dopamine buffer solution, react at room temperature for 20 h, rinse with distilled water and ethanol, and dry at room temperature for 24 h before use.

[0031] Step 2: MIL-160 film preparation

[0032]Dissolve 0.2g of aluminum trichloride hexahydrate, 0.26g of 2,5-furandicarboxylic acid, and 0.12g of sodium formate in 15g of distilled water, stir magnetically until the solution is clear, and then stir overnight to prepare MIL-160 membrane synthesis solution; Pour the synthesis solution into the reaction kettle with the dopamine-modified porous alumina substrate in step 1. After the reaction kettle was sealed, it was placed in an oven a...

Embodiment 3

[0034] MIL-160 films were synthesized as follows:

[0035] Step 1: Modification of Porous Alumina Matrix by Dopamine Functionalization

[0036] With embodiment 1 step 1.

[0037] Step 2: MIL-160 film preparation

[0038] Dissolve 0.2g of aluminum trichloride hexahydrate, 0.26g of 2,5-furandicarboxylic acid, and 0.08g of sodium hydroxide in 15g of distilled water, magnetically stir until the solution is clear, and then stir overnight to prepare MIL-160 film synthesis liquid; pour the synthesis liquid into the reactor with the dopamine-modified porous alumina substrate in step 1. After the reaction kettle was sealed, it was placed in an oven and reacted at 100° C. for 24 hours. After the reaction, take it out, rinse it with distilled water, and dry it at room temperature.

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Abstract

The invention discloses a metal-organic framework MIL-160 film, a preparation method and an application, and belongs to the technical field of preparation of functional film separating materials. Themetal-organic framework MIL-160 film has excellent chemical stability and hydrothermal stability, the hole diameter of the film is about 0.6 nanometer, and the size of the hole diameter is equal to that of the dynamics diameter of a xylene homologue. According to the method, a porous aluminum oxide substrate is functionally modified through dopamine, polydopamine is modified on the surface of theporous substrate, MIL-160 particle 'capturing' and 'adsorbing' capacity of the surface of the porous substrate is enhanced, so that nucleating and growing of the MIL-160 film on the surface of the substrate are facilitated, and the uniform and compact MIL-160 film is prepared and has high separation performance. The MIL-160 film prepared by the method is used for separation of xylene geometric isomers, the xylene permeation flux of the film is 258-563g*m<-2>*h<-1>, and the p-xylene / o-xylene separation coefficient of the film is 16.8-38.5 at the pervaporation temperature of 25-100 DEG C.

Description

technical field [0001] The invention belongs to the field of preparation of membrane separation materials, in particular to a method for synthesizing metal organic framework membranes widely used in gas separation and liquid separation, and in particular to provide a uniform and dense membrane with excellent xylene isomerism prepared by functional modification of dopamine Metal-organic framework membrane MIL-160 membrane with volume separation performance and its preparation method. Background technique [0002] Xylene is the main component of C8 aromatics, and there are three isomers (p-xylene PX, o-xylene OX, m-xylene MX). P-xylene is an important chemical raw material for the synthesis of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT). Para-xylene, as part of BTX aromatics (benzene, toluene and xylene isomers), must be separated from ortho-, meta-, and ethylbenzene by distillation, adsorption, crystallization, and reaction processes. However, due ...

Claims

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Application Information

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IPC IPC(8): B01D61/36B01D67/00B01D71/06C07C7/144C07C15/08
CPCB01D61/362B01D67/0006B01D71/06C07C7/144C07C15/08
Inventor 黄爱生吴小草马习习黄思诺
Owner EAST CHINA NORMAL UNIVERSITY
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