A metal-organic framework mil-160 film and its 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, defects, pinhole intergranular, etc., and achieve high selective separation performance , the effect of high separation performance

Active Publication Date: 2021-05-07
EAST CHINA NORMAL UNIV
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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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  • A metal-organic framework mil-160 film and its preparation method and application
  • A metal-organic framework mil-160 film and its preparation method and application
  • A metal-organic framework mil-160 film and its 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 membrane, a preparation method and application thereof, and belongs to the preparation technology of functional membrane separation materials. The metal organic framework MIL‑160 membrane has excellent chemical stability and hydrothermal stability, the pore size is about 0.6 nm, and the pore size is comparable to the kinetic diameter of xylene homologues. The method of the present invention first uses dopamine to functionalize the porous alumina matrix, and a layer of polydopamine is modified on the surface of the porous matrix to enhance the "capture" and "adsorption" ability of the surface of the porous matrix to MIL-160 particles, thereby promoting MIL-160 The membrane nucleates and grows on the surface of the substrate to prepare a uniform and dense MIL‑160 membrane with high separation performance. The MIL-160 membrane prepared by this method is used for the separation of xylene isomers, and at the pervaporation temperature of 25-100°C, the permeation flux of p-xylene is 258-563 g m ‑2 h ‑1 , The separation coefficient of p / o-xylene is 16.8-38.5.

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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Patent Type & Authority Patents(China)
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 UNIV
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