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Preparation method for temperature-sensitive separation membrane with nanometer ordered aperture

A sensitive film and pore size technology, which is applied in semipermeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve the problem of inconspicuous response performance of temperature-sensitive membranes, and achieve simple and efficient pore-forming process, improved response speed, and responsive The effect of process synergy

Inactive Publication Date: 2013-12-25
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) The block copolymer PS-b-PNIPAAm was synthesized in two steps by atom transfer radical method. Specifically: place 0.1g CuBr, 0.27gα,α′-bipyridine (BPY) and 0.1g initiator ethyl 2-bromopropionate at the bottom of the reaction flask, then add 15ml styrene and 3ml toluene, freeze in liquid nitrogen for 10 minutes minutes, vacuumize, fill with nitrogen, thaw at room temperature, and repeat 2-3 times. The reaction was carried out 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, wash with ethanol precipitation, and repeat the dissolution and precipitation three times. The product was dried under vacuum at 40°C for 12h.

[0024] Add 0.125g CuBr, 3g macroinitiator PS-Br, 0.25ml Me to the reaction flask 6 TREN, 3g of NIPAAm and 6ml of solvent DMF, frozen in liquid nitrogen for 10 minutes, vacuumed, filled with...

Embodiment 2

[0028] (1) The block copolymer PS-b-PNIPAAm was synthesized in two steps by atom transfer radical method. Specifically: place 0.1g CuBr, 0.27gα,α′-bipyridine (BPY) and 0.1g initiator ethyl 2-bromopropionate at the bottom of the reaction flask, then add 15ml styrene and 3ml toluene, freeze in liquid nitrogen for 10 minutes minutes, vacuumize, fill with nitrogen, thaw at room temperature, and repeat 2-3 times. The reaction was carried out 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, wash with ethanol precipitation, and repeat the dissolution and precipitation three times. The product was dried under vacuum at 40°C for 12h.

[0029] Add 0.125g CuBr, 3g macroinitiator PS-Br, 0.25ml Me to the reaction flask 6 TREN, 3g of NIPAAm and 6ml of solvent DMF, frozen in liquid nitrogen for 10 minutes, vacuumed, filled with...

Embodiment 3

[0033] (1) The block copolymer PS-b-PNIPAAm was synthesized in two steps by atom transfer radical method. Specifically: place 0.1g CuBr, 0.27gα,α′-bipyridine (BPY) and 0.1g initiator ethyl 2-bromopropionate at the bottom of the reaction flask, then add 15ml styrene and 3ml toluene, freeze in liquid nitrogen for 10 minutes minutes, vacuumize, fill with nitrogen, thaw at room temperature, and repeat 2-3 times. The reaction was carried out at 110°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, wash with ethanol precipitation, and repeat the dissolution and precipitation three times. The product was dried under vacuum at 50°C for 12h.

[0034] Add 0.125g CuBr, 3g macroinitiator PS-Br, 0.25ml Me to the reaction flask 6 TREN, 3g of NIPAAm and 6ml of solvent DMF, frozen in liquid nitrogen for 10 minutes, vacuumed, filled with...

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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 a technology for preparing an intelligent polymer material, in particular to a block copolymer of synthesizing polystyrene (PS) and poly-N-isopropylacrylamide (PNIPAAm), which is selectively swollen by a block copolymer-based material Pore-forming method to prepare highly ordered, temperature-sensitive nanoporous films. By spin coating or dip coating, nanoporous thin films are prepared on the surface of commercial separation base membranes, and temperature-sensitive composite membranes with fast response speed and precise separation performance are prepared. 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 biomimetic materials, and it is the future development direction of membrane materials. The so-called intelligent separation membrane is a separation membrane whose structure and properties (such as...

Claims

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Application Information

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