A kind of graft type polyionic liquid polyimide membrane and preparation method thereof
A technology of polyionic liquids and polyimide membranes, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve problems such as high selectivity, high permeability coefficient, and inability to overcome the trade-off effect, and achieve The effect of good film-forming properties and good solubility properties
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Embodiment 1
[0041] Synthesis of diamine monomer: under nitrogen protection, 9ml of trifluoromethanesulfonic acid was added to a 50mL three-necked flask, and 0.735g (5mmol) of indoline-2,3-dione was added to dissolve it. Slowly add 1.80ml (20mmol) aniline under the condition of the bath, remove the ice bath after stirring for ten minutes, and then react at room temperature for 8h. The reaction solution was neutralized to alkaline with 2M NaOH solution, extracted with dichloromethane, the oil phase was rotary evaporated, and gel chromatography was separated with a developer with a dichloromethane:methanol molar ratio of 10:1, and then the product was rotary evaporated again, Vacuum drying was performed at 100° C. for 12 hours to obtain monomer powder.
[0042] Preparation of polyimide polymer: under nitrogen protection, add 30ml m-cresol solvent into a 100ml three-necked flask, weigh 1.577g (5mmol) iminodiamine monomer to dissolve, and then add 2.221g (5mmol) in four batches 6FDA was stirr...
Embodiment 2
[0050] The synthesis of diamine monomer: with embodiment 1
[0051] Preparation of polyimide polymer: under nitrogen protection, add 30ml m-cresol solvent into a 100ml three-necked flask, weigh 1.577g (5mmol) of iminodiamine monomer to dissolve, and then add 1.091g (5mmol) in four batches Stir pyromellitic dianhydride at room temperature for 10 minutes, gradually raise the temperature to 180°C and react for 8 hours, cool to room temperature, precipitate the obtained polymer into excess methanol, wash repeatedly, and vacuum dry at 60°C for 12 hours to obtain a polymer product.
[0052] Preparation of grafted polyionic liquid material: Add 25ml of anhydrous DMF into a 50ml single-necked flask, dissolve 3.8g (5mmol) of polyimide in the solvent, add 1.064g (7.5mmol) of methyl iodide and seal the vial away from light React at 80°C for 30 hours, cool to room temperature and precipitate the obtained polymer in excess ether. After repeated washing several times, vacuum dry at 80°C for ...
Embodiment 3
[0058] The synthesis of diamine monomer: with embodiment 1
[0059] Preparation of polyimide polymer: under nitrogen protection, add 30ml m-cresol solvent into a 100ml three-necked flask, weigh 1.577g (5mmol) iminodiamine monomer to dissolve, and then add 1.551g (5mmol) in four batches Stir diphenyl ether tetracarboxylic dianhydride at room temperature for 10 minutes, gradually raise the temperature to 180°C and react for 8 hours, cool to room temperature, precipitate the obtained polymer in excess methanol, wash repeatedly, and vacuum dry at 60°C for 12 hours to obtain a polymer product.
[0060] Preparation of grafted polyionic liquid material: Add 25ml of anhydrous DMF into a 50ml single-necked flask, dissolve 3.8g (5mmol) of polyimide in the solvent, add 1.064g (7.5mmol) of methyl iodide and seal the vial away from light React at 80°C for 30 hours, cool to room temperature and precipitate the obtained polymer in excess ether. After repeated washing several times, vacuum d...
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