Molecularly imprinted mixed ligand lanthanide trimetal-organic framework and preparation method thereof
A mixed ligand and molecular imprinting technology, which is applied in the direction of material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of low detection limit and insufficient sensitivity, and achieve the effects of low detection limit, simple preparation method and low cost
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Embodiment 1
[0022] Preparation method of molecularly imprinted mixed ligand lanthanide trimetal-organic framework (one-pot method)
[0023] 1) 450 mg of gadolinium nitrate hexahydrate Gd (NO 3 ) 3 ·6H 2 O, 3mg europium nitrate hexahydrate Eu (NO 3 ) 3 ·6H 2 O, 0.1mL0.3g / L terbium nitrate hexahydrate Tb(NO 3 ) 3 ·6H 2 O, 254mg 1,2,4,5-benzenetetracarboxylic acid (H 4 BETC), 180 mg of 2,5-furandicarboxylic acid (H 2 FDA), 5 mL methanol and 40 mL water were added to a 100 mL round bottom flask, and refluxed at 95°C for 4 hours;
[0024] 2) Filter and wash the obtained white powder with water and methanol, and air dry naturally.
Embodiment 2
[0026] Preparation of crystalline materials (step-by-step method):
[0027] 1) 450 mg of gadolinium nitrate hexahydrate Gd (NO 3 ) 3 ·6H 2 O, 3mg europium nitrate hexahydrate Eu (NO 3 ) 3 ·6H 2 O, 0.1mL0.3g / L terbium nitrate hexahydrate Tb(NO 3 ) 3 ·6H 2 O, 254mg 1,2,4,5-benzenetetracarboxylic acid (H 4 BETC), 180 mg of 2,5-furandicarboxylic acid (H 2 FDA) was dissolved in a mixed solvent of 15 mL of N,N-dimethylformamide and 25 mL of water, 8 mL of the above solution was added to a 20 mL vial, and reacted at 95°C for 5 hours to obtain a transparent strip-shaped mixed ligand lanthanide Crystals of trimetal-organic framework (NKU-66-EuGdTb);
[0028] 2) Put 460 mg of NKU-66-EuGdTb crystals into methanol at 50 °C for 72 hours and exchange them repeatedly to obtain a molecularly imprinted mixed ligand lanthanide trimetal-organic framework (NKU-66-EuGdTb-P) with template removal. crystals;
[0029] 3) Wash the obtained crystals with water and air dry naturally.
Embodiment 3
[0031] Characterization:
[0032] Get the crystal (NKU-66-EuGdTb) obtained in the above-mentioned embodiment 2 on the glass slide, select the suitable crystal under the microscope, carry out the test on the XtaLAB Mini II type X-ray single crystal diffractometer, use the graphite monochromatic Monochromated Mo-Kα rays is the incident radiation source, with The diffraction points were collected by scanning, their coordinates and their anisotropy parameters were corrected by the least square method, and the positions of hydrogen atoms were obtained by theoretical hydrogenation. All calculations were performed using the SHELXTL package. The crystal structure was analyzed by Olex-2 software, combined with the results of elemental analysis, inductively coupled plasma resonance and thermogravimetric analysis, the molecular formula of NKU-66-EuGdTb-P powder was finally determined as {[Eu 0.0067 Gd 0.992 Tb 0.0013 (BETC) 0.5 (FDA) 0.5 (H 2 O) 2 ]·0.25CH 3 OH 2H 2 O} n , w...
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