Polyimide nanofiber composite membrane, preparation method and application of polyimide nanofiber composite membrane in organic solvent nanofiltration process
A polyimide and nanofiber technology, applied in the field of separation membranes, can solve problems such as the permeability limitation of asymmetric basement membranes
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[0045] A new technical route for preparing organic solvent-resistant nanofiltration membranes is proposed in the present invention: the insoluble PI nanofibrous base membrane is produced by electrospinning polyamic acid (PAA) followed by thermal imidization, and then adopts hydrophilic A water-based intermediate layer is used to assist in the preparation of a dense selective layer on a hydrophobic base film.
[0046] The resulting thin film nanofiber composite (TFNC) membrane has a rejection rate of 98.4% of Janus Green B (MW: 511.07Da), and a pure THF flux of 4.61Lm -2 h -1 bar -1 , the pure water flux is 22.44Lm -2 h -1 bar -1 . Thin film composite (TFC) membranes have enhanced stability in polar aprotic solvents such as dimethylformamide (DMF), dimethylsulfoxide (DMSO), and tetrahydrofuran (THF), highlighting their use in Potential applications in enhancing polar solvent separations.
Embodiment 1
[0047] The preparation of embodiment 1 insoluble PI nanofiber base film PI nanofiber base film manufacture
[0048] (1) Electrospun nanofibrous membranes from a PAA precursor solution prepared by polycondensation of 4,4'-diaminodiphenyl ether (ODA) and equimolar pyromellitic anhydride (PMDA) in DMF of. A predetermined amount of 4,4'-diaminodiphenyl ether (ODA) and equimolar pyromellitic anhydride (PMDA) were dispersed in DMF in a three-necked flask with a solid content of 20 wt%. The mixture was mechanically stirred at 25°C for 4 hours to obtain a homogeneous PAA solution, and left to stand for 12 hours to eliminate trapped air bubbles in the solution.
[0049] (2) Prepare the nanofibrous membrane by electrospinning the PAA solution: by applying the optimal voltage (19.0kV) and flow rate (1.0mLh -1 ), the width (20.0mm) and the tip-to-collector distance (16.0cm) under the electric field, the PAA solution was electrospun onto the aluminum foil to prepare the PI nanofiber memb...
Embodiment 2PI
[0051] The preparation of embodiment 2PIP-PEI-TFNC film
[0052] First, the surface of the nanofiber base film prepared in Example 1 was exposed to an aqueous solution (2.0% w / w) of polyethyleneimine (PEI, Mw ~ 70k) for 10 minutes, and then mixed with 0.1% w / w Tricarboyl chloride (TMC) / n-hexane was used for crosslinking for 2 minutes, and after forming the PEI crosslinked intermediate layer, the surface of the nanofiber-based membrane was exposed to PIP aqueous solution (1% w / w) for 2 minutes. Excessive PIP solution was removed from the base film using a rubber roller, and then exposed to a hexane solution containing 0.1% w / w TMC for 2 minutes to carry out the cross-linking reaction. The resulting PIP-PEI-TFNC membranes were washed several times with deionized water and finally stored in ethanol at room temperature before being characterized.
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