Preparation method of mixed matrix membrane based on porous core-shell filler
A technology of mixed matrix membranes and fillers, which is applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve the problems of reduced gas selectivity and weak interaction, and achieve improved selectivity, controllable reactions, and preparation processes. simple effect
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[0040] The preparation method of ZIF-8@AC comprises the following steps:
[0041] Step1: Add 0.84g MgCl2·6(H2O) into 20mL ethanol at room temperature, sonicate for 1h until it is completely dissolved to obtain a mixed solution;
[0042] Step2: Add 1.3 mL of 3-aminopropyltriethoxysilane (APTES) dropwise to the above-mentioned dissolved solution under the condition of magnetic stirring, and stir it overnight;
[0043] Step3: Based on the above steps, the precipitate was collected by centrifugation, washed three times with ethanol, and then dried in a vacuum oven at a drying temperature of 60°C for 24 hours to obtain an amino clay (AC) filler;
[0044] Step4: Weigh 0.02 g of the AC filler obtained above and dissolve it in 5 mL of hydroalcoholic solution (60 / 40, v / v) at room temperature, then adjust the pH of the solution to neutral to obtain neutral sexual solution;
[0045] Step5: Add 0.117g of Zn(NO3)2 6(H2O) to the neutral solution, sonicate for 1h until completely dissolved, ...
Embodiment 1
[0060] The Pebax / ZIF-8@AC-3 mixed matrix membrane was prepared. The thickness of the mixed matrix membrane was 98 μm. The mixed matrix membrane used Pebax as the membrane matrix, and ZIF-8@AC was added to the membrane matrix. Among them, Pebax and ZIF- The mass ratio of 8@AC is 0.97:0.03, and the preparation method of the mixed matrix membrane is as follows:
[0061] Step 1. Preparation of ZIF-8@AC:
[0062] Add 0.84g MgCl2 6H2O into 20mL ethanol at room temperature, sonicate for 1h until it dissolves completely. Then, under the condition of magnetic stirring, 1.3 mL of 3-aminopropyltriethoxysilane (APTES) was dropped into the above-mentioned dissolving solution dropwise, and stirred overnight. Finally, the precipitate was collected by centrifugation, washed three times with ethanol, and dried in a vacuum oven at 60°C for 24 hours to obtain an amino clay (AC) filler.
[0063] Weigh 0.02 g of the AC filler obtained above and dissolve it in 5 mL of hydroalcoholic solution (60 / ...
Embodiment 2
[0069] Prepare Pebax / ZIF-8@AC-5 mixed matrix membrane, the difference from Example 1 Pebax / ZIF-8@AC-3 mixed matrix membrane is: the thickness of the membrane is 101 μm, wherein, Pebax and ZIF-8@AC The mass ratio is 0.95:0.05. The difference between the preparation of the mixed matrix membrane and the preparation method of Example 1 is that in step 3, the weighing of 0.0162g ZIF-8@AC is changed to weighing of 0.027g ZIF-8@AC; Finally, a mixed matrix membrane with a thickness of 101 μm was obtained. figure 2 It is a scanning electron microscope sectional view of the Pebax / ZIF-8@AC-5 mixed matrix membrane prepared in Example 2.
[0070] Under the conditions of 25°C and 2bar, the Pebax / ZIF-8@AC-5 mixed matrix membrane prepared in Example 2 was used for the separation test of CO2 / CH4 mixed gas with a CO2 volume fraction of 20% under wet conditions. The CO2 flux is 516 Barrer and the CO2 / CH4 selectivity is 30.
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