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Composite separation membrane based on in situ growth organic framework structure of fluorine-containing copolymer and its preparation method and application

An organic framework and in-situ growth technology, applied in separation methods, semi-permeable membrane separation, dispersed particle separation, etc., can solve the problem of low selectivity of separation membrane materials, overcome the inability to prepare large areas, and achieve interface matching and The effect of close compatibility

Active Publication Date: 2022-02-11
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above-mentioned problems existing in the prior art, the object of the present invention is to provide a kind of physical properties such as excellent selective separation, high temperature resistance, swelling resistance and high strength, based on perfluoro-2,2-dimethyl-1, 3-dioxole-tetrafluoroethylene-amino-terminated olefin ternary random copolymer in-situ grown composite separation membrane material with an organic framework structure and its preparation method to overcome the selectivity of existing separation membrane materials low-level defects

Method used

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  • Composite separation membrane based on in situ growth organic framework structure of fluorine-containing copolymer and its preparation method and application
  • Composite separation membrane based on in situ growth organic framework structure of fluorine-containing copolymer and its preparation method and application
  • Composite separation membrane based on in situ growth organic framework structure of fluorine-containing copolymer and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 140g of perfluoroheptane and 40g of perfluoroisopropanol into the autoclave, seal the nitrogen flow and exhaust oxygen until the oxygen concentration is less than 5ppm, and 0.084 moles (mol) of perfluoro-2,2-dimethyl -1,3-dioxole (PDD), 0.006mol of 4-penten-1-amine, and 0.038mol of tetrafluoroethylene were respectively added to the reaction kettle, and after stirring evenly, 0.53 Millimoles (mmol) of diisopropyl peroxydicarbonate (dissolved in 20g perfluoroheptane), stirred evenly and heated up to 50°C, polymerized for 6h, cooled to normal temperature, and unreacted tetrafluoroethylene monomer was removed, After the reaction, the solution was washed with tetrahydrofuran and methanol, and precipitated to obtain poly(perfluoro-2,2-dimethyl-1,3-dioxole-tetrafluoroethylene-4 -pentene-1-amine) random copolymer; after vacuum drying for 24h, take 0.2g of poly(perfluoro-2,2-dimethyl-1,3-dioxolane which can be further modified by reaction ene-tetrafluoroethylene-4-penten-1-...

Embodiment 2

[0034] Add 130g of hexafluorobenzene and 50g of perfluoroisopropanol into the reactor, seal the nitrogen and discharge oxygen until the oxygen concentration is less than 5ppm, and add 0.082mol of perfluoro-2,2-dimethyl-1,3- Dioxole (PDD), 0.006mol of 5-hexen-1-amine, and 0.026mol of tetrafluoroethylene were added to the reaction kettle respectively, and after stirring evenly, 0.55 mmol of diperoxide was added by a booster pump. Diisopropyl carbonate (dissolved in 20g hexafluorobenzene), stir well and heat up to 45°C, polymerize for 8 hours, cool to room temperature, remove unreacted tetrafluoroethylene monomer, wash the reacted solution with tetrahydrofuran and methanol respectively , precipitation, to obtain a ternary random copolymer that can be further modified by reaction; after vacuum drying for 24 hours, take 0.1 g of a ternary random copolymer that can be further modified by reaction and 1.9 g of poly(perfluoro-2,2 -Dimethyl-1,3-dioxol-co-tetrafluoroethylene) copolymer ...

Embodiment 3

[0040]Add 130g of perfluoroheptane and 50g of perfluoroisopropanol into the reaction kettle, seal the nitrogen and discharge oxygen until the oxygen concentration is less than 5ppm, and add 0.102mol of perfluoro-2,2-dimethyl-1,3 - Dioxole (PDD), 0.014mol of 4-penten-1-amine, and 0.025mol of tetrafluoroethylene were added to the reaction kettle, and after stirring evenly, 0.68mmol of peroxide was added by a booster pump. Diisopropyl dicarbonate (dissolved in 20g perfluoroheptane), stirred evenly and heated to 45°C, polymerized for 8 hours, cooled to normal temperature, excluded unreacted tetrafluoroethylene monomer, and passed the reaction solution through tetrahydrofuran, Methanol washing and precipitation, to obtain a ternary random copolymer that can be further modified by reaction; after vacuum drying for 24 hours, take 0.1 g of a ternary random copolymer that can be further modified by reaction and 1.9 g of poly(perfluoro-2 , 2-Dimethyl-1,3-dioxole-co-tetrafluoroethylene) ...

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Abstract

The invention discloses a composite separation membrane based on an in-situ grown organic framework structure of a fluorine-containing copolymer, a preparation method and an application thereof. Random copolymerization of a certain proportion of perfluoro-2,2-dimethyl-1,3-dioxole (PDD), tetrafluoroethylene (TFE) and amino-terminated olefins can be further modified by reaction fluorine-containing copolymers, mixed with PDD-co-TFE binary copolymers in different proportions, and formed into membranes, through the Schiff base reaction, the covalent organic framework structure sheets are grown in situ on the surface of the membrane substrate, and the functional The group is introduced into the framework structure to form a coordination structure, and a fluorine-containing copolymer composite separation membrane is obtained. The composite separation membrane prepared by the method of the present invention significantly enhances the binding force between the fluorine-containing copolymer layer and the organic framework structure layer through amine bridging, and realizes the adjustable internal pore size through the internal structure modification of the pores of the organic framework structure layer , can efficiently and selectively separate organic gases and inorganic gases (oxygen, carbon dioxide, etc.), and has extremely high practical value.

Description

technical field [0001] The invention belongs to the field of chemical engineering and technology, and in particular relates to a composite separation membrane based on an in-situ growth organic framework structure of a fluorine-containing copolymer, a preparation method and application thereof. Background technique [0002] Due to its high free volume fraction and good gas permeability, poly(perfluoro-2,2-dimethyl-1,3-dioxole-co-tetrafluoroethylene) (P(PDD- co-TFE)) copolymers have a wide range of applications in the field of gas separation membranes. Poly(perfluoro-2,2-dimethyl-1,3-dioxole-co-tetrafluoroethylene) is currently mainly produced by DuPont Company of the United States, and its trade name is AF, and divided into different grades according to the PDD content and molecular weight of the copolymer, the most commonly used varieties are AF1600 and AF2400. The US patent "US3978030 Fluorinated Dioxin Polymer" disclosed for the first time the method of preparing perfl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D69/12B01D67/00B01D71/44B01D53/22
CPCB01D69/125B01D71/44B01D53/228
Inventor 余大洋郑威包永忠蔡怀勋王树华
Owner ZHEJIANG UNIV
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