A kind of preparation method and application of ionic liquid and metal organic framework composite adsorbent
A technology of metal-organic frameworks and ionic liquids, which is applied in separation methods, chemical instruments and methods, and separation of dispersed particles. It can solve the problems of limiting the industrial application of ionic liquids, high viscosity of ionic liquids, and high energy consumption for desorption and regeneration. It can be designed Strong resistance, high hydrothermal stability and acid and alkali resistance, and the effect of improving selectivity
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Embodiment 1
[0043] MIL-101 can be prepared according to the existing published literature methods, specifically: add 4.00g of chromium nitrate nonahydrate, 1.64g of terephthalic acid, 125μL of hydrofluoric acid and 70mL of water into a 100mL reaction kettle, and sonicate for 3h. React at 220°C for 8 hours to obtain unpurified MIL-101 crystals. After cooling, the unpurified MIL-101 was sequentially treated with hot water at 80°C for 5h, hot ethanol at 60°C for 3h, ammonium fluoride at 60°C for 10h, and finally washed with hot water ultrasonically for 5 times. It is to remove the terephthalic acid ligand remaining in the channel. The purified product was vacuum-dried at 80°C and 150°C for 12h and 5h, respectively, to obtain the purified MIL-101 as a green solid powder. The specific surface area is 3000m 2 / g, the pore volume is 1.5cm 3 / g(P / P 0 = 0.95). Unless otherwise specified, the following examples are MIL-101 synthesized by this method.
[0044] After testing, at 298K, under 100...
Embodiment 2
[0046] Preparation of the adsorbent [Bmim][OAc]@MIL-101: Accurately weigh 0.5500g of [Bmim][OAc] and dissolve it in 5mL of chromatographically pure ethanol. in ethanol. Then, 150 mg of purified MIL-101 was added to the above solution, and the stirring was continued for 24 h. Green solid powder was obtained by suction filtration, and vacuum-dried at 80°C for 12 hours to obtain [Bmim][OAc]@MIL-101 with a loading capacity of 1.0 mmol / g.
[0047] After testing, at 298K and 100kPa, the adsorption capacity of the adsorbent prepared in this example is 2.0mmol / g for acetylene, and 0.84mmol / g for ethylene, and IAST calculates C 2 h 2 / C 2 h 4 (1:1) separation selectivity is 6.7; at 273K, 100kPa, the adsorption capacity of acetylene is 3.0mmol / g, the adsorption capacity of ethylene is 1.5mmol / g, IAST calculation C 2 h 2 / C 2 h 4 (1:1) separation selectivity was 7.9.
Embodiment 3
[0049] Preparation of adsorbent [Bmim][OAc]@MIL-101: Accurately weigh 0.0500g of [Bmim][OAc] and dissolve it in 5mL of chromatographically pure ethanol. in ethanol. Then, 150 mg of purified MIL-101 was added to the above solution, and the stirring was continued for 24 h. Green solid powder was obtained by suction filtration, and vacuum-dried at 80°C for 12 hours to obtain [Bmim][OAc]@MIL-101 with a loading capacity of 0.1 mmol / g.
[0050] After testing, at 298K and 100kPa, the adsorption capacity of the adsorbent prepared in this example is 2.5mmol / g for acetylene and 1.3mmol / g for ethylene, and IAST calculates C 2 h 2 / C 2 h 4 (1:1) separation selectivity is 3.2; at 273K, 100kPa, the adsorption capacity of acetylene is 4.1mmol / g, the adsorption capacity of ethylene is 2.3mmol / g, IAST calculation C 2 h 2 / C 2 h 4 (1:1) separation selectivity was 3.7.
[0051] figure 1 It is the XRD characterization diagram of MIL-101 prepared in Example 1 and [Bmim][OAc]@MIL-101 prep...
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