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Method for preparing functional polymer micro-porous membrane with reaction-solution phase inversion control method

A solution phase inversion, functional polymer technology, which is applied in the field of the preparation of crown ether grafted polymer microporous membranes by the reaction-controlled immersion precipitation phase inversion method, can solve the problems of poor controllability of membrane structure, insoluble and infusible polymers, etc. Chemical modification resistance and other problems, to achieve the effect of improved fracture strength, mild operating conditions and high porosity

Inactive Publication Date: 2016-07-27
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The modification of the base film after film formation has the following disadvantages and deficiencies: the uniformity of modification is poor, and only the inner and outer surfaces of the film can be modified; The property effect is poor; the modification after film formation will further change the formed film structure, and the controllability of the film structure will become poor.
However, in the preparation process of polymer microporous membranes, in order to obtain a larger amount of crown ether grafted polysulfone polymer microporous membranes, due to the degree of reaction during the grafting reaction of amino crown ethers and chloromethyl polysulfones Gel phenomenon occurs when the size is too large, making the polymer insoluble and infusible, and cannot be formed into a film by conventional non-solvent-induced phase inversion method

Method used

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  • Method for preparing functional polymer micro-porous membrane with reaction-solution phase inversion control method
  • Method for preparing functional polymer micro-porous membrane with reaction-solution phase inversion control method
  • Method for preparing functional polymer micro-porous membrane with reaction-solution phase inversion control method

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Experimental program
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Effect test

Embodiment 1

[0026] Reaction-controlled phase inversion method to prepare 4-aminobenzo-15-crown 5 grafted polysulfone microporous membrane, specifically as follows: Weigh 3g chloromethylated polysulfone (chloromethyl substitution degree is 20%) and dissolve in 57mlDMF After completely dissolving, add 1.9g of 4-aminobenzo-15-crown-5 ether to it, react at 45°C for 22 hours, then vacuum defoam at 20°C, then apply the casting solution on a glass plate, place the glass plate on In coagulation bath water (20° C.), take out and dry after coagulation and molding for 30 minutes, and prepare 4-aminobenzo-15-crown 5 grafted polysulfone polymer microporous membrane. The polymer microporous membrane prepared under the above conditions was circulated and adsorbed 100mL0.5mol / L lithium iodide solution under 0.05MPa pressure at 20°C for 30 minutes to obtain 4-aminobenzo-15-crown 5-grafted polysulfone polymer microporous membrane. The pore membrane separation factor was 1.035.

Embodiment 2

[0028]Reaction-controlled phase inversion method to prepare 4-aminobenzo-15-crown 5 grafted polyethersulfone microporous membrane, specifically as follows: Weigh 3g of chloromethylated polyethersulfone (chloromethyl substitution degree is 50%) and dissolve After completely dissolving in 57ml of DMF, add 1.9g of 4-aminobenzo-15-crown-5 ether to it, react at 45°C for 15h, then vacuum degassing at 20°C, and then apply the casting solution on a glass plate. The plate was placed in coagulation bath water (20° C.), and after solidification and molding for 30 minutes, it was taken out and dried to prepare a 4-aminobenzo-15-crown 5 grafted polyethersulfone polymer microporous membrane. The polymer microporous membrane prepared under the above conditions was circulated and adsorbed 100mL0.5mol / L lithium iodide solution under 0.05MPa pressure at 20°C for 30 minutes to obtain 4-aminobenzo-15-crown 5-grafted polyethersulfone polymer The microporous membrane separation factor was 1.040.

Embodiment 3

[0030] Reaction-controlled phase inversion method to prepare 4-aminobenzo-12-crown 4 grafted polysulfone microporous membrane, specifically as follows: Weigh 3g chloromethylated polysulfone (chloromethyl substitution degree is 20%) and dissolve in 57mlDMF After completely dissolving, add 1.7g of 4-aminobenzo-15-crown-5 ether to it, react at 45°C for 22 hours, then vacuum defoam at 20°C, then apply the casting solution on a glass plate, place the glass plate on In coagulation bath water (20° C.), take out and dry after coagulation and molding for 30 minutes, and prepare 4-aminobenzo-15-crown 5 grafted polysulfone polymer microporous membrane. The polymer microporous membrane prepared under the above conditions was circulated and adsorbed 100mL0.5mol / L lithium iodide solution under 0.05MPa pressure at 20°C for 30 minutes to obtain 4-aminobenzo-12-crown-4 grafted polysulfone polymer microporous membrane. The pore membrane separation factor was 1.035.

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Abstract

The invention belongs to the technical field of functional polymer membrane separation, and relates to a method for preparing a crown-ether graft polymer micro-porous membrane with a reaction-solution phase inversion control method. The method includes the steps that a chloromethyl-containing polymer such as polysulfone or polyether sulfone or polyether ether ketone is dissolved into a reaction solvent, an active-amido containing crown ether compound such as 4-aminobenzene-15-crown-5 is added, and a crown ether graft polymer is prepared through a nucleophilic substitution reaction between chloromethyl and amino; the grafting ratio of the reaction is controlled; in other words, when a reaction system is in certain viscosity, the reaction is terminated to prevent gelatinizing, the reaction system at the moment serves as a membrane casting solution, and the crown-ether graft polymer micro-porous membrane is prepared with the solution phase inversion method. As a cross bond exists in the polymer system, it can be achieved that the polymer micro-porous membrane which is high in porosity ratio and breaking strength is prepared under the low solid content of the polyether, and the separation step and the purification step of the grafted polymer are omitted; as a crown ether group exists, the polymer membrane has excellent lithium isotope separation performance.

Description

technical field [0001] The invention belongs to the technical field of separation of functional polymer membranes, in particular to a method for preparing crown ether grafted polymer microporous membranes by a reaction-controlled immersion precipitation phase inversion method. Background technique [0002] Membrane separation technology is a high-tech developed in the mid-1960s. It uses a separation membrane with separation and selective permeation as the filter medium, and uses the principles of sieving of membrane pores, charge effects, and dissolution and diffusion to separate the solute and the solute in the mixture. Methods of solvent separation, fractionation, extraction and enrichment. Compared with ordinary filter media, the separation membrane has controllable pore size and narrower pore size distribution, and higher separation accuracy. The phase inversion method is the most commonly used method for preparing polymer microporous membranes or composite membrane bas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/20C08G75/23C08J5/18B01D71/68B01D69/02B01D67/00
CPCC08G75/20B01D67/0002B01D69/02B01D71/68B01D2323/36B01D2325/02C08G75/23C08J5/18C08J2381/06
Inventor 李建新裴洪昌严峰崔振宇
Owner TIANJIN POLYTECHNIC UNIV
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