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A method for preparing a temperature-sensitive separation membrane with nano-ordered pores

A technology of sensitive membrane and pore size, applied in semi-permeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve the problem of insignificant response performance of temperature-sensitive membrane, achieve simple and efficient pore-forming process, synergistic response process, and responsive The effect of increased speed

Inactive Publication Date: 2015-12-23
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This leads to the inconspicuous response performance of this type of temperature sensitive film.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Block copolymer PS-b-PNIPAAm was synthesized in two steps by atom transfer radical method. Specifically: 0.1g CuBr, 0.27g α, α'-bipyridine (BPY) and 0.1g initiator 2-ethyl bromopropionate were placed at the bottom of the reaction flask, then 15ml styrene and 3ml toluene were added, and liquid nitrogen was frozen for 10 Minutes, vacuumize, fill with nitrogen, and thaw at room temperature, repeat 2-3 times like this. React at 110°C for 24h. After the reaction was completed, it was rapidly cooled to 0°C. Dissolve with an appropriate amount of dichloromethane, remove CuBr by suction filtration, pass through a neutral alumina column, and then wash with ethanol precipitation, and dissolve the precipitate three times repeatedly. The product was dried under vacuum at 40 °C for 12 h.

[0024] Add 0.125g CuBr, 3g macromolecular initiator PS-Br, 0.25ml Me 6 TREN, 3g NIPAAm and 6ml solvent DMF were frozen in liquid nitrogen for 10 minutes, vacuumized, filled with nitrogen, ...

Embodiment 2

[0028] (1) Block copolymer PS-b-PNIPAAm was synthesized in two steps by atom transfer radical method. Specifically: 0.1g CuBr, 0.27g α, α'-bipyridine (BPY) and 0.1g initiator 2-ethyl bromopropionate were placed at the bottom of the reaction flask, then 15ml styrene and 3ml toluene were added, and liquid nitrogen was frozen for 10 Minutes, vacuumize, fill with nitrogen, and thaw at room temperature, repeat 2-3 times like this. React at 130°C for 24h. After the reaction was completed, it was rapidly cooled to 0°C. Dissolve with an appropriate amount of dichloromethane, remove CuBr by suction filtration, pass through a neutral alumina column, and then wash with ethanol precipitation, and dissolve the precipitate three times repeatedly. The product was dried under vacuum at 40 °C for 12 h.

[0029] Add 0.125g CuBr, 3g macromolecular initiator PS-Br, 0.25ml Me 6 TREN, 3g NIPAAm and 6ml solvent DMF were frozen in liquid nitrogen for 10 minutes, vacuumized, filled with nitrogen, ...

Embodiment 3

[0033] (1) Block copolymer PS-b-PNIPAAm was synthesized in two steps by atom transfer radical method. Specifically: 0.1g CuBr, 0.27g α, α'-bipyridine (BPY) and 0.1g initiator 2-ethyl bromopropionate were placed at the bottom of the reaction flask, then 15ml styrene and 3ml toluene were added, and liquid nitrogen was frozen for 10 Minutes, vacuumize, fill with nitrogen, and thaw at room temperature, repeat 2-3 times like this. React at 1I0°C for 48h. After the reaction was completed, it was rapidly cooled to 0°C. Dissolve with an appropriate amount of dichloromethane, remove CuBr by suction filtration, pass through a neutral alumina column, and then wash with ethanol precipitation, and dissolve the precipitate three times repeatedly. The product was dried under vacuum at 50 °C for 12 h.

[0034] Add 0.125g CuBr, 3g macromolecular initiator PS-Br, 0.25ml Me 6 TREN, 3g NIPAAm and 6ml solvent DMF were frozen in liquid nitrogen for 10 minutes, vacuumized, filled with nitrogen, ...

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Abstract

A new preparation technology, which is a segmented-copolymer selective swelling pore-forming method, is utilized for preparation of a temperature-sensitive membrane with nanometer ordered aperture, and a composite membrane with a temperature-responding surface is prepared by coating or spin coating of the temperature-sensitive membrane on a conventional basic membrane material. The temperature-sensitive membrane has uniform membrane aperture dimension, and consistent content and distribution of aperture surface PNIPAAm, and is capable of effectively improving response performance of the temperature-sensitive membrane. The preparation method of the temperature-sensitive membrane mainly comprises the following steps: synthesizing a segmented copolymer PS-b-PNIPAAm by utilizing an atom transfer free-radical method, dissolving SP-b-PNIPAAm and performing spin coating on SP-b-PNIPAAm on the surface of a clean glass sheet, drying, performing solvent annealing, placing the annealed glass sheet in ethanol or water for swelling pore-forming to obtain the polymer membrane with nanometer ordered aperture. The PS-b-PNIPAAm / PP(PVDF) composite membrane with a surface layer possessing a nanometer porous temperature-responding functional layer is obtained by utilizing the method which comprises that a commercial basic membrane (PP / PVDF) is coated by the PS-b-PNIPAAm solution by a spin mode.

Description

technical field [0001] The invention relates to the preparation technology of intelligent polymer materials, specifically a block copolymer of polystyrene (PS) and poly-N-isopropylacrylamide (PNIPAAm), which is selectively swollen by the block copolymer base material A highly ordered, temperature-sensitive nanoporous film is prepared by a pore-forming method. A nanoporous film is prepared on the surface of a commercial separation base membrane by spin coating or dip coating to obtain a temperature sensitive composite membrane with fast response speed and precise separation performance. It belongs to the field of membrane technology. Background technique [0002] Environmentally responsive smart membrane is a new type of functional membrane developed based on bionic materials, and it is the future development direction of membrane materials. The so-called intelligent separation membrane is a separation membrane whose structure and performance (such as pore size, hydrophilic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/80B01D67/00
Inventor 冯霞王倩李战陈莉赵义平
Owner TIANJIN POLYTECHNIC UNIV