Method for preparing solvent-resistant and acid-alkali-resistant homoporous membrane through crosslinking

A technology of acid and alkali resistance and solvent resistance, which is applied in the field of cross-linking preparation of homoporous membranes

Active Publication Date: 2021-02-02
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cross-linked homoporous membrane exhibits good solvent resistance and strong acid and alkali resistance, which overcomes the problem that the existing polymer-based homoporous membrane cannot be used in organic solvents, strong acids and alkalis.

Method used

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  • Method for preparing solvent-resistant and acid-alkali-resistant homoporous membrane through crosslinking
  • Method for preparing solvent-resistant and acid-alkali-resistant homoporous membrane through crosslinking
  • Method for preparing solvent-resistant and acid-alkali-resistant homoporous membrane through crosslinking

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Preparation of homoporous membrane: the PS-b-P4VP block copolymer with a molecular weight of 210,000g / mol, wherein PS accounts for 71wt%, is dissolved in N, N dimethylformamide / 1,4 dioxane / tetrahydrofuran = 4:3:3 mixed solvent, stir until uniformly dissolved, after standing for a period of time, apply it to a clean glass plate with a scraper with a thickness of 150 μm, volatilize for 15 seconds, and then immerse in water Phase inversion to form a film. After the solvent exchange is complete, the formed film is taken out and dried to obtain a homoporous film. The electron microscope characterizes its structure, see attached figure 1 The original membrane picture in the upper left corner of .

[0033] (2) Cross-linking reaction and post-treatment: immerse the film prepared above into a 0.5 g / ml ferric chloride / formaldehyde dimethyl acetal cross-linking agent solution, heat and react at 60°C for 6 hours, take out the film after reaction, and use Rinse 3 times with et...

Embodiment 2

[0040](1) Preparation of homoporous membrane: PS-b-P4VP block copolymer with a molecular weight of 100,000g / mol, in which PS accounts for 75wt%, is dissolved in 1,4 dioxane / tetrahydrofuran at a concentration of 25wt% / dimethylformamide = 4.9:2.1:3 mixed solvent, stir until uniformly dissolved, after standing for a period of time, use a scraper with a thickness of 150 μm to coat a clean glass plate, volatilize for 90 seconds, and then immerse in water for phase transformation into Membrane, after the solvent exchange is complete, the formed film is taken out and dried to obtain a homoporous membrane, and the homoporous structure on the surface is characterized by electron microscopy.

[0041] (2) Cross-linking reaction and post-treatment: immerse the film prepared above into a 0.25 g / mol aluminum trichloride / formaldehyde dimethyl acetal cross-linking agent solution, react at 20°C for 12 hours, take out the film after reaction, Rinse three times with ethanol, rinse once with ac...

Embodiment 3

[0046] (1) Preparation of homoporous membrane: PS-b-PAA block copolymer with a molecular weight of 150,000g / mol, in which PS accounts for 84wt%, is dissolved in 1,4-dioxane at a concentration of 22wt% , stir until it dissolves evenly, after standing for a period of time, use a scraper with a thickness of 150 μm to coat it on a clean glass plate, immerse in water after volatilization for 10 seconds to form a phase conversion film, and after the solvent exchange is complete, take out the formed film and dry it to obtain Homoporous film, electron microscope characterizes its homogeneous surface structure, see figure 1 The first picture of the second row.

[0047] (2) Cross-linking reaction and post-treatment: immerse the film prepared above into a 5g / ml ferric chloride / dimethyl acetal cross-linking agent solution, heat and react at 80°C for 6h, and wash the film after reaction with ethanol for 3 times , washed with acetic acid for 3 times, then transferred to dimethyl sulfoxide ...

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Abstract

The invention discloses a method for preparing a solvent-resistant and acid-alkali-resistant homoporous membrane by crosslinking, which comprises the following steps: carrying out phase inversion on ablock copolymer material containing benzene rings as hydrophobic chain segments to obtain a homoporous membrane, and treating the homoporous membrane with a solvent-free crosslinking agent solution to crosslink the benzene rings, thereby finally forming the solvent-resistant and acid-alkali-resistant homoporous membrane. According to the method, a new block copolymer with a reactive functional group does not need to be adopted, and all block copolymer films containing benzene rings can be cross-linked by additionally adding a cross-linking agent. The method has the advantages of mild crosslinking reaction conditions, simple steps and high universality, and is beneficial to large-scale production of the solvent-resistant homoporous membrane. The prepared homogeneous pore membrane providespossibility for precise separation in an organic solvent environment.

Description

technical field [0001] The invention belongs to the field of special separation materials, and in particular relates to a cross-linking preparation method of a uniform-porous membrane resistant to solvents and acid and alkali. Background technique [0002] Homoporous membrane refers to a separation membrane with uniform pore size and uniform pore type. The unique structure endows it with the ability of precise separation. In recent years, the method of preparing homoporous membranes based on block copolymers has been extensively studied. Among them, the homoporous membrane is prepared by combining the self-assembly characteristics of the block copolymer with the phase inversion, which makes the large-scale preparation of the homoporous membrane possible, which lays the foundation for the scale-up production and commercial application of the homoporous membrane. [0003] In recent years, organic solvents have been widely used in paint, medicine, chemical industry, printing ...

Claims

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Application Information

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IPC IPC(8): B01D71/82B01D69/02B01D67/00
CPCB01D71/82B01D69/02B01D67/0093B01D67/0006B01D67/0011B01D2325/02B01D2325/30
Inventor 易砖王文静杨草英吴涛
Owner ZHEJIANG UNIV OF TECH
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