A kind of microporous polymer composite membrane and preparation method thereof
A polymer and composite membrane technology, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve problems such as inability to achieve large-scale industrial production, heterogeneous composite membrane structure, and agglomeration of microporous and nanomaterials, and achieve the The method is simple and easy to control, with high repeatability and stable performance.
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Embodiment 1
[0033] Step 1: Dissolve 10g PIM-1 in 200mL tetrahydrofuran, stir for 24 hours to fully dissolve, then let stand for 2 hours until the solution is transparent, and filter impurities.
[0034] Step 2: Take 20 mL of the solution obtained in Step 1 into a sample bottle, add 0.01 g of 1,4-diacetophenone, ultrasonicate for 20 min, and stir for 30 min.
[0035] Step 3: Take 10 mL of the uniform solution in step 2 in an ultra-flat petri dish at the bottom, and after the solvent evaporates for 48 hours, peel off the membrane from the petri dish to obtain a mixed matrix membrane PIM-1 / M1-1%; Dry overnight in a vacuum oven at 80°C.
[0036] Step 4: Submerge the dried PIM-1 / M1-1% membrane obtained in Step 3 in methanesulfonic acid for 10 minutes, take it out, and drain excess methanesulfonic acid.
[0037] Step 5: Put the film obtained in Step 4 into a high-temperature oven at 110° C. for 48 hours to undergo a cross-linking reaction to obtain a PIM-1 / PPN1-1% cross-linked film.
[0038] ...
Embodiment 2
[0042] Step 1: Dissolve 10g PIM-1 in 200mL tetrahydrofuran, stir for 24 hours to fully dissolve, then let stand for 2 hours until the solution is transparent, and filter impurities.
[0043] Step 2: Take 20 mL of the solution obtained in Step 1 in a sample bottle, add 0.03 g of 1,4-diacetophenone, ultrasonicate for 20 min, and stir for 30 min.
[0044] Step 3: Take 10 mL of the homogeneous solution in step 2 in an ultra-flat petri dish at the bottom, and after the solvent evaporates for 48 hours, peel off the membrane from the petri dish to obtain a mixed matrix membrane PIM-1 / M1-3%; Dry overnight in a vacuum oven at 80°C.
[0045] Step 4: Submerge the dried PIM-1 / M1-3% membrane obtained in Step 3 into methanesulfonic acid for 10 minutes, take it out, and drain excess methanesulfonic acid.
[0046] Step five: put the film obtained in step four into a high-temperature oven at 110° C. for 48 hours to undergo a cross-linking reaction to obtain a PIM-1 / PPN1-3% cross-linked film. ...
Embodiment 3
[0051] Step 1: Dissolve 10g PIM-1 in 200mL tetrahydrofuran, stir for 24 hours to fully dissolve, then let stand for 2 hours until the solution is transparent, and filter impurities.
[0052] Step 2: Take 20 mL of the solution obtained in Step 1 in a sample bottle, add 0.05 g of 1,4-diacetophenone, ultrasonicate for 20 min, and stir for 30 min.
[0053] Step 3: Take 10 mL of the homogeneous solution in step 2 in an ultra-flat petri dish at the bottom, and after the solvent evaporates for 48 hours, peel off the membrane from the petri dish to obtain a mixed matrix membrane PIM-1 / M1-5%; Dry overnight in a vacuum oven at 80°C.
[0054] Step 4: Submerge the dried PIM-1 / M1-5% membrane obtained in Step 3 into methanesulfonic acid for 10 minutes, take it out, and drain excess methanesulfonic acid.
[0055] Step 5: Put the film obtained in Step 4 into a high-temperature oven at 110° C. for 48 hours to undergo a crosslinking reaction to obtain a PIM-1 / PPN1-5% crosslinked film.
[0056...
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