A kind of preparation method of homogeneous membrane

A technology of porous membrane and solution, applied in the field of preparation of phenolic resin homoporous membrane, can solve the problems of incomplete removal of template agent, need special equipment, limited application scope, etc. good order effect

Active Publication Date: 2017-11-10
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can remove the template agent better, it often requires higher temperature and harsher conditions; especially for organic-organic materials, it will inevitably cause the shrinkage of the pores and the separation of functional groups when removing the template agent. At the same time, most of them become inorganic carbon materials after high-temperature calcination, which greatly limits its application range, especially in the field of separation membranes.
However, other methods for removing templates have been widely concerned by researchers, such as microwave digestion, supercritical fluid extraction, etching, solvent extraction and other methods. Compared with direct calcination methods, these methods often have template removal Incomplete, tedious and time-consuming, and require special equipment

Method used

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  • A kind of preparation method of homogeneous membrane
  • A kind of preparation method of homogeneous membrane
  • A kind of preparation method of homogeneous membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 0.10g of sodium hydroxide aqueous solution to 0.47g of molten phenol and stir evenly, add 0.81g of formaldehyde solution and react the solution at 60°C for 2h, adjust the solution to be neutral with hydrochloric acid solution; after drying, the phenolic resin prepolymer will be obtained Dissolve 1.26g of block copolymer F127 in 10.0g of water to obtain a solution; transfer the solution to a petri dish, and after the solvent is completely evaporated, heat and cure for 1 hour to obtain a composite film of phenolic resin and block copolymer; The composite membrane was placed in a 1,2-dichloroethane solution with a molar concentration of 0.5% of 1,4-p-dichlorobenzyl and a molar concentration of anhydrous ferric chloride of 1.0%, and was heated to 40°C for 24 hours.

[0039] figure 1 It is the SEM picture of the phenolic resin homoporous membrane prepared in this example. It can be seen from the figure that the membrane prepared in this example has an ordered two-dimens...

Embodiment 2

[0047]Add 0.10g of sodium hydroxide aqueous solution into 0.47g of molten phenol and stir evenly, add 0.81g of formaldehyde solution and react the solution at 70°C for 1.25h, adjust the solution to be neutral with hydrochloric acid solution; after drying, the prepolymerized phenolic resin will be obtained The body and 0.58g block copolymer P123 were dissolved in 10.0g methanol to obtain a solution; the solution was transferred to a petri dish, and after the solvent was completely volatilized, it was heated and solidified for 12 hours to obtain a composite film of phenolic resin and block copolymer; The obtained composite membrane was placed in a dimethylformamide solution with a molar concentration of 1,4-dibromobutane of 1.5% and anhydrous aluminum chloride of 5.0%, and was heated to 60°C for 12 hours.

[0048] Figure 7 It is the SEM image of the phenolic resin homoporous membrane prepared in this example. It can be seen from the figure that the homoporous membrane prepared...

Embodiment 3

[0055] Add 0.10g of sodium hydroxide aqueous solution into 0.47g of molten phenol and stir evenly, add 0.81g of formaldehyde solution and react the solution at 90°C for 2 hours, adjust the solution to be neutral with hydrochloric acid solution; after drying, the phenolic resin prepolymer will be obtained Dissolve 1.10 g of block copolymer F108 in 10.0 g of ethanol to obtain a solution; transfer the solution to a petri dish, and after the solvent is completely volatilized, heat and cure for 24 hours to obtain a composite film of phenolic resin and block copolymer; The obtained composite membrane was placed in a dimethyl sulfoxide solution with a molar concentration of 1,4-terephthaloyl chloride of 2.5% and anhydrous tin tetrachloride of a molar concentration of 3.0%, and was heated to 80°C for 5 hours.

[0056] SEM figure, TEM figure, SAXS spectrogram, N 2 The analysis results of the adsorption-desorption isotherm diagram, pore size distribution curve diagram and FT-IR diagram ...

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Abstract

The invention belongs to the technical field of porous material separation membranes and discloses a preparation method of a polymer homopore membrane. A polyoxyethylene-polyoxypropylene-polyoxyethylene block copolymer is taken as a template, resole is taken as a precursor, a compound adopting a regular structure is formed through self-assembly, and then aromatic dihalide or alkane dihalide is taken as a cross-linking agent, so that benzene rings in phenolic resin have a Friedel-Crafts reaction to be further cross-linked. In the reaction process, produced byproduct hydrogen halide removes a template, so that pores are formed during crosslinking, the homopore membrane is prepared with the one-step method. The homopore membrane prepared with the method has orderly arranged pore channels and uniform pore diameter and height, takes highly crosslinked phenolic resin as the framework and has good high-temperature resistance, acid and base resistance and organic solvent resistance. Raw materials are cheap and easy to obtain, equipment is simple, the preparation technology process is short, independent template removing and pore forming steps are not needed, and the preparation method is suitable for mass production and has bright application prospect in fields of separation, adsorption, heat insulation and the like.

Description

technical field [0001] The invention belongs to the technical field of porous material separation membranes, and in particular relates to a preparation method of a phenolic resin homoporous membrane. Background technique [0002] Homoporous membranes are porous materials with ordered channels and uniform pore size, and have important application values ​​in the fields of separation, catalysis, adsorption, and biomedicine. The template method is a widely used method for preparing homoporous membranes, which can be divided into hard template method and soft template method. The hard template method usually uses silicon-based materials as templates to replicate the established structure in reverse phase; while the soft template method uses block copolymers or surfactants as templates to self-assemble with organic precursors to form an ordered structure. Flexible and convenient, the shape and material itself can be effectively regulated according to the difference of the soft t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/80B01D67/00B01D69/02
CPCB01D67/0006B01D69/02B01D71/80B01D2323/12B01D2323/18B01D2323/30B01D2323/38B01D2325/22B01D2325/30
Inventor 汪勇霍西康邢卫红汪朝晖
Owner NANJING TECH UNIV
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