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Method for preparing metal-organic framework UiO-66 series membranes and separating methanol/methyl tert-butyl ether mixture

A metal-organic framework, uio-66 technology, applied in the separation/purification of hydroxyl compounds, semi-permeable membrane separation, ether separation/purification, etc. Improved crystallinity and high permeation flux

Active Publication Date: 2017-03-15
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the mesoporous fiber carrier used is a self-made carrier, and the membrane-making method is not universal; Liu et al [Liu J, Canfield N, Liu W. Preparation and Characterization of a Hydrophobic Metal-Organic Framework Membrane Supported on a Thin Porous Metal Sheet[ J].Industrial&Engineering ChemistryResearch.2016,55(13):3823–3832]Synthesized UiO-66-CH on porous nickel mesh 3 membrane, and applied to CO 2 Separation, but no attempt at liquid separation

Method used

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  • Method for preparing metal-organic framework UiO-66 series membranes and separating methanol/methyl tert-butyl ether mixture
  • Method for preparing metal-organic framework UiO-66 series membranes and separating methanol/methyl tert-butyl ether mixture
  • Method for preparing metal-organic framework UiO-66 series membranes and separating methanol/methyl tert-butyl ether mixture

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Experimental program
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Embodiment 1

[0021] 1. Preparation of UiO-66 film

[0022] (1) Carrier pretreatment:

[0023] α-Al with a pore size of 0.2 μm 2 o 3 The ceramic tube carrier was vibrated in ultrasonic with acetone and ethanol, then rinsed with deionized water several times, vibrated ultrasonically, and dried at 100°C for later use.

[0024] (2) Preparation and implantation of UiO-66 seed crystals

[0025] Zirconium tetrachloride (ZrCl 4 ), terephthalic acid (H 2 BDC), glacial acetic acid (CH 3 COOH) and N,N-dimethylformamide (DMF) as raw materials, respectively weighed 0.0746g zirconium tetrachloride, 0.0532g terephthalic acid, 80ml N,N-dimethylformamide, 2.25ml glacial acetic acid , mixed and stirred for 30 minutes to prepare the UiO-66 seed crystal precursor solution, and injected into a stainless steel crystallization kettle with a polytetrafluoroethylene lining, sealed and placed in an oven at 120°C for 24 hours before taking it out to obtain a particle size of 100-150nm The pure UiO-66 seed cry...

Embodiment 2

[0031] 1. UiO-66-NH 2 Membrane preparation

[0032] (1) Carrier pretreatment:

[0033] α-Al with a pore size of 0.2 μm 2 o 3 The ceramic tube carrier was vibrated in ultrasonic with acetone and ethanol, then rinsed with deionized water several times, vibrated ultrasonically, and dried at 100°C for later use.

[0034] (2)UiO-66-NH 2 Seed preparation

[0035] Zirconium tetrachloride (ZrCl 4 ), aminoterephthalic acid (H 2 BDC-NH 2 ), glacial acetic acid (CH 3 COOH) and N,N-dimethylformamide (DMF) as raw materials, weigh 0.0746g zirconium tetrachloride, 0.0580g aminoterephthalic acid, 80ml N,N-dimethylformamide, 2.25ml ice Acetic acid, formulated UiO-66-NH 2 Seed precursor. Stir at room temperature for 30 minutes, pour into a stainless steel crystallization kettle lined with polytetrafluoroethylene, seal it and place it in an oven at 120°C, and take it out after 24 hours. Obtain pure UiO-66-NH with a particle size of 100-150nm 2 The seed crystal is prepared into an aq...

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Abstract

The invention provides a method for preparing metal-organic framework UiO-66 series membranes and separating a methanol / methyl tert-butyl ether mixture and belongs to the technical field of chemical separation. According to the method, the metal-organic framework UiO-66 series membranes are growth and synthesized through putting a porous ceramic tube carrier with a seed layer into a membrane forming solution; through adding a glacial acetic acid regulator, the forming of continuous and complete high-performance membranes is facilitated. The methanol / methyl tert-butyl ether mixture is effectively separated by using the screening performance and methanol preferential adsorbability of the UiO-66 series membranes, and the UiO-66 series membranes have good stability in a separation system. According to the method, by making full use of the screening performance and methanol preferential adsorption characteristic of the UiO-66 series membranes, the permeation flux is relatively high and is higher than 1.2kg / (m<2>h), the separation effect is good, the separating factor is greater than 200, and the permeation performance can be kept stable in long-term operation, so that the practical application value is potential.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and relates to a method for permeating and evaporating a methanol / methyl tert-butyl ether mixture with a stable metal-organic framework UiO-66 series membrane. Background technique [0002] Methyl tert-butyl ether (MTBE) is an important raw material for the preparation of high-purity isobutene, and is widely used as an additive and reaction solvent for unleaded gasoline. MTBE is generally synthesized by the addition of methanol and isobutene in the C4 fraction. This reaction is a reversible reaction. In order to ensure a high conversion rate of isobutene, it is necessary to add excess methanol, and excess methanol will form an azeotrope with the generated MTBE ( Methanol mass fraction is 14.3%). The traditional separation method is water washing-distillation process, which requires complex equipment and huge energy consumption. Replacing this traditional separation process with memb...

Claims

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Application Information

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IPC IPC(8): B01D71/06B01D69/04B01D69/02B01D67/00B01D61/36C07C41/36C07C43/04C07C29/76C07C31/04
CPCB01D61/362B01D67/0002B01D69/02B01D69/04B01D71/06B01D2325/36C07C29/76C07C41/36C07C43/04C07C31/04
Inventor 张雄福吴飞超刘海鸥
Owner DALIAN UNIV OF TECH
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