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Composite separation membrane based on fluorine-containing copolymer and having in-situ grown organic framework structure and preparation method and application of composite separation membrane

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: 2021-08-06
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 fluorine-containing copolymer and having in-situ grown organic framework structure and preparation method and application of composite separation membrane
  • Composite separation membrane based on fluorine-containing copolymer and having in-situ grown organic framework structure and preparation method and application of composite separation membrane
  • Composite separation membrane based on fluorine-containing copolymer and having in-situ grown organic framework structure and preparation method and application of composite separation membrane

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 a fluorine-containing copolymer and having an in-situ grown organic framework and a preparation method and application of the composite separation membrane. The preparation method comprises the following steps: randomly copolymerizing perfluoro-2,2-dimethyl-1,3-dioxole (PDD), tetrafluoroethylene (TFE) and amine-terminated olefin according to a certain ratio to prepare a fluorine-containing copolymer which can be further subjected to reaction modification; mixing the fluorine-containing copolymer with a PDD-co-TFE binary copolymer according to different ratios to prepare a membrane; and performing Schiff base reaction to grow a covalent organic frame structure sheet layer in situ on the surface of a membrane matrix and introducing a functional group into a frame structure to form a coordination structure so as to obtain the fluorine-containing copolymer composite separation membrane. According to the composite separation membrane prepared by the method disclosed by the invention, binding force between a fluorine-containing copolymer layer and an organic framework structure layer is remarkably enhanced through amino bridging, and the adjustability of an internal pore size is realized through the modification of the internal structure of the pore channel of the organic framework structure layer, so organic gas and inorganic gas (oxygen, carbon dioxide and the like) can be efficiently and selectively separated; and the method 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 Applications(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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