A kind of nh2-mil-125/pod-cooh ultra-thin homogeneous hybrid forward osmosis membrane and preparation method thereof
A technology of NH2-MIL-125 and POD-COOH, applied in chemical instruments and methods, semi-permeable membrane separation, permeation/dialysis water/sewage treatment, etc., can solve damage, poor mechanical strength, and eliminate concentration difference in the support layer Polarization and other issues, to achieve the effect of broad application prospects, high water permeability, excellent water permeability and salt retention performance
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[0035] The invention provides a kind of NH 2 -The preparation method of MIL-125 / POD-COOH ultra-thin homogeneous hybrid forward osmosis membrane, specifically comprising:
[0036] Step 1: Add butyl titanate and 2-amino-terephthalic acid to a mixed solution of N,N-dimethylformamide (DMF) and methanol, stir at room temperature for 3 to 5 hours, then transfer to 40 ml In a polytetrafluoroethylene-lined stainless steel reaction kettle, place it in a temperature-programmed oven at 140-150°C for 24-48 hours. After naturally cooling to room temperature, wash with N,N-dimethylformamide (DMF) for 3 to 5 times and then with methanol for 3 to 5 times, each solution is 20 to 30 ml, and the time is 2 to 3 hours , to obtain MOFs material NH 2 -MIL-125;
[0037] Step 2: Hydrazine sulfate (N 2 h 4 ·H 2 SO 4 ) and polyphosphoric acid (PPA) were added to a three-neck flask equipped with a mechanical stirrer, a nitrogen vent, a thermometer, a Dean-Stark water dispenser and a condenser tube...
Embodiment 1
[0054] 1) Butyl titanate (0.84 mL, 0.75 mmol) and 2-amino-terephthalic acid (1.5 g, 3 mmol) were added to 10 mL of N,N-dimethylformamide (DMF) and methanol in the mixed solution (V (DMF) :V (甲醇) 1:1), stirred at room temperature for 3 hours, transferred to a 40 ml polytetrafluoroethylene-lined stainless steel reaction kettle, and placed in a temperature-programmed oven at 150°C for 24 hours. After naturally cooling to room temperature, wash with N,N-dimethylformamide (DMF) for 3 times and then with methanol for 3 times, each solution is 20 ml for 2 hours, and then put into Dry in a vacuum oven at 150°C for 12 hours to obtain the MOFs material NH 2 -MIL-125. figure 2 The MOFs material NH prepared for Example 1 of the present invention 2 -XRD pattern of MIL-125, such as figure 2 As shown, the five peaks at 6.8°, 9.8°, 11.6°, 16.6°, 17.6° and 17.9° in the XRD pattern of the synthesized MOF particles are respectively attributed to (101), (200), (211) , (222) and (312) crys...
Embodiment 2
[0061] 1) the method described in 1) of embodiment 1 makes NH 2 -MIL-125 material.
[0062] 2) Polyoxadiazole material (POD) was prepared by the method described in 2) of Example 1.
[0063] 3) The method described in 3) of Example 1 makes carboxyl-containing polyoxadiazole material (POD-COOH)
[0064] 4) Dissolve the above-mentioned carboxyl-containing polyoxadiazole material (0.5 g, 0.002 mole) in 30 ml of anhydrous DMF solvent. After the polymer is completely dissolved, it is added dropwise to the solution containing EDC (0.068 g, 0.355 mmol) , NHS (0.0035 g, 0.03 mmol) and NH 2 -In 5 milliliters of anhydrous DMF of MIL-125 material (0.05 g), about 2 hours after the dropwise addition is completed, continue to stir at room temperature for 72 hours, and discharge in n-hexane to obtain 10% NH 2 - MIL-125 / POD-COOH hybrid material.
[0065] 5) The 10% NH prepared above 2 -The MIL-125 / POD-COOH hybrid material was dissolved in DMF solvent to ensure that the mass fraction of t...
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