Membrane preparation method for simultaneously constructing nanopore structure and surface electrical properties
A nanoporous structure and electrical technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of limited membrane performance, low degree of crosslinking by modifier method, gelation, etc. build effect
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[0064] The preparation method of the present invention is suitable for preparing polymer separation membranes containing imide functional groups, and the polymer containing imide described here can refer to: polyetherimide, polyimide, polyamideimide (PAI); their molecular structures are as follows:
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[0069] The modifying agent used in the present invention is a polymer containing amine groups, such as polyethyleneimine, as long as it is a modifying agent containing amine groups. Such as ethylenediamine, triethylamine, hexamethylenediamine, triethylenetetramine, etc.
[0070] In order to avoid the gelation phenomenon of the polymer and the modifier reacting in advance during the premixing process, the reactive functional groups of the modifier were pre-protected before blending.
[0071] The protective agent used here is mainly the amine-based protective agent, mainly the amine-based protective agent of the carbonyl system, such ...
Embodiment 1
[0072] Embodiment 1 polyethyleneimine pre-protection
[0073] With a molecular weight of 1800 g mol -1 Polyethyleneimine (PEI 1800 ) preprotection reaction as an example. 5 g PEI 1800 and 10.4 g di-tert-butyl dicarbonate (Boc) 2 O was separately dissolved in dichloromethane (DCM) to prepare 20 wt% PEI 1800 and 20wt% (Boc) 2 O solution. Subsequent to (Boc) 2 O solution was slowly added to PEI dropwise 1800 The solution was stirred at 25°C for 12 hours and a milky white dispersion was collected. Centrifuge at 10,000 rpm and wash three times with dimethylacetamide (DMAc) to remove DCM to obtain the composite, named PEI 1800 - Boc, where 1800 represents the molecular weight of polyethyleneimine.
[0074] In the above process, how to precisely control PEI and (Boc) 2 The ratio of O is a difficult problem to be solved because PEI has a complex polymer structure with different types of amine groups. (Boc) 2 O not only protects primary amines (-NH 2 ), can also protect s...
Embodiment 2
[0084] The preparation of embodiment 2 separation membrane
[0085] Intact cortical asymmetric membranes (ISAs) were prepared using a non-solvent-induced phase inversion method. The dried polyimide (Extem ® ) was dissolved in DMAc according to a certain proportion, stirred at 65°C for 8 hours, according to the concentration of 26 wt% Extem ® / DMAc binary system solution, and then cooled to 25°C. Subsequently, the PEI-Boc additive (PEI with a molecular weight of 1800 in Example 1) was added to the polymer solution so that the content of the additive in the polymer solution was 4 wt%, stirred at 25°C for 8 h, and then left to stand for 12 hour defoaming. After doctor blade coating with a scale of 150 μm, the film was immersed in a coagulation bath with 1 mol / L hydrochloric acid; after that, the film was transferred to a pure water bath at 70°C and heated for 10 minutes. Finally, the membranes were removed from the thermal bath and stored in pure water for later use. The prep...
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