Mixed matrix membrane containing imidazolate metal-organic framework material and its preparation and application
A technology of imidazolate metal and mixed matrix membrane, which is applied in the field of membrane separation, can solve the problem of low compatibility between particle agglomeration and polymer phases, and achieve the effect of improving membrane separation performance, good compatibility, and improving separation performance
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[0037] The invention provides a method for preparing a mixed matrix film containing imidazole ester metal organic framework material, which comprises the following steps:
[0038] S1: Mix the N,N-dimethylformamide (DMF) solution of the imidazole ligand containing the aldehyde group with the DMF solution of zinc acetate, stir and react for a period of time at room temperature, centrifuge and freeze dry;
[0039] S2: Put the freeze-dried imidazole metal organic framework material (ZIF-OH) containing aldehyde group into a methanol flask, add the reducing agent and reflux for a period of time at 60°C, and centrifuge to obtain imidazole metal containing hydroxyl group The organic framework material (ZIF-CHO) material is redispersed in methanol solution for use;
[0040] S3: Mix the methanol dispersion liquid of the imidazole ester metal organic framework material (ZIF-CHO) containing hydroxyl, polydimethylsiloxane (PDMS), crosslinking agent and catalyst raw materials to form a casting liq...
Embodiment 1
[0052] In a 250mL round bottom flask, add a solution of 0.845g imidazole-2-formaldehyde in 50mL DMF, then add 0.964g zinc acetate, stir at 65°C for 60min, centrifuge, wash with methanol several times, freeze-dry 1 day. The initial measurement ratio of the whole reaction n(Zn 2+ The molar ratio of ):n (imidazole-2-carboxaldehyde) is 1:2, and the product ZIF-90 is finally obtained.
[0053] Weigh 1.2g of synthesized ZIF-90 into the flask, then add 50ml of methanol and stir at 60℃ for 1 hour. After the suspension is uniform, add 0.6g of sodium borohydride, continue to stir for 24 hours and centrifuge to obtain the product ZIF-91 , Re-disperse in methanol solution for later use.
[0054] The raw materials containing ZIF-91 nanoparticles, polydimethylsiloxane (PDMS), crosslinking agent, and catalyst are mixed in a mass ratio of 1:10:1:0.05 to form a casting liquid, and after stirring, vacuum degassing 2h, finally pour the casting solution on the prepared PVDF base film, scrape the fil...
Embodiment 2
[0056] In a 250 mL round bottom flask, add 0.845 g imidazole-5-formaldehyde in 50 mL DMF solution, then add 1.308 g zinc nitrate dissolved in it, stir at 65°C for 60 min, centrifuge, wash several times with methanol, freeze dry 1 day. The initial measurement ratio of the whole reaction n(Zn 2+ The molar ratio of ):n (imidazole-5-carboxaldehyde) is 1:3, and the product ZIF-CHO is finally obtained.
[0057] Weigh 1.2g of synthesized ZIF-CHO into the flask, then add 50ml of methanol and stir at 60℃ for 1 hour, add 0.6g of potassium borohydride after the suspension is uniform, continue stirring for 24h, and centrifuge to obtain the product ZIF-OH , Re-disperse in methanol solution for later use.
[0058] The raw materials containing ZIF-OH nanoparticles, polymethylphenylsiloxane (PMPS), cross-linking agent, and catalyst are mixed in a mass ratio of 2:10:1:0.05 to form a casting solution. After stirring, it is vacuumed off. Soak for 2h, and finally pour the casting solution on the fin...
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