Polycrystalline metal-organic framework membranes for separating mixtures
An organic framework, polycrystalline metal technology, applied in the field of polycrystalline metal-organic framework film, can solve the problems of low packing density, chemical tunability limited application and so on
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Embodiment 1
[0166] Example 1: Preparation and characterization of Sm-DOBDC films
[0167] Defect-free Sm-BOBDC membranes were fabricated on alumina hollow fibers by a secondary growth method.
[0168] Preparation of Sm-DOBDC Films
[0169] Polycrystalline Sm-DOBDC membranes were fabricated on the outer surface of porous alumina ceramic hollow fibers by secondary growth synthesis. The alumina support sealed at both ends was placed in a PTFE holder, and the immersion molar composition was 1Sm (NO 3 ) 3 : 1.5 DOBDC: 500 DMF / ethanol: 70 in the mother liquor of 2-FBA.
[0170] Crystallization was performed in a Teflon-lined stainless steel autoclave at 105°C for (1+3) days (in situ growth: 1 day, secondary growth: 3 days). Specifically, the culture was performed at 105° C. for 24 h (1 day) in a Teflon-lined stainless steel autoclave. In this culture, Sm-DOBDC nanocrystals were seeded on the outside of the support. After cooling to room temperature, the seeded Sm-DOBDC membranes were th...
Embodiment 2
[0180] Example 2: Pervaporation-based separation of alcohol / water mixtures using Sm-DOBDC membranes
[0181] The separation performance of Sm-DOBDC membranes as prepared according to Example 1 was evaluated by alcohol dehydration based on pervaporation.
[0182] Experimental setup and calculations
[0183] using a homemade device ( Figure 5 ) to evaluate membrane performance by pervaporation for separation of water from aqueous organics. One end of the membrane is sealed with silicone and the other open end is assembled in the module. The effective length (approximately 25 mm) and diameter of the membrane are accurately measured. The Sm-DOBDC hollow fiber membrane was immersed in the previously prepared alcohol / water mixture, and the pressure on the permeate side was maintained at about 250 Pa.
[0184] The system was given 10 min for stabilization before samples were collected. Permeate vapor was collected with a cold trap equipped with liquid nitrogen. The alcohol c...
Embodiment 3
[0229] Example 3: In situ repair of Sm-DOBDC films
[0230] The possibility of in-situ repair in Sm-DOBDC films is demonstrated to address defect formation during operation of polycrystalline films.
[0231] process
[0232] By immersing the freshly prepared membranes in 80 wt.% water / ethanol solution (pH=2) for a period of time (up to 35 h, see experimental details in the next paragraph) to mimic possible membrane degradation during long-term operation in a corrosive environment, to prepare partially degraded Sm-DOBDC films. In situ repair ( Figure 8 a).
[0233] To elaborate on the repair process, degraded Sm-DOBDC membranes were placed in 20 mL scintillation vials filled with supernatant that could be collected repeatedly during membrane preparation or repair. Then, the membrane was incubated at 105°C for 2100 min (35 h). Finally, the repaired membranes were washed three times with DMF and ethanol, respectively, and then activated overnight in a fume hood.
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