A Membrane Forming Method Simultaneously Constructing Nanopore Structure and Surface Electricity
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, difficult interaction, low crosslinking degree of modifier method, etc., and achieve high efficiency Construction, precise and selective separation capabilities, excellent results in water flux
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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 20 wt% (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 ...
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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