A cage polysilsesquioxane/metal-2-aminoterephthalic acid organic framework hybrid material and its preparation method
A technology of aminoterephthalic acid and polysilsesquioxane, applied in chemical instruments and methods, other chemical processes, water/sewage treatment, etc., can solve problems such as difficult processing and difficult deviceization, and solve processing difficulties , Facilitate processing, and solve the effect that it is not easy to device
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[0057] Metal ion is Zr 4+ The preparation method of MOFs with the structure shown in Formula I of ion clusters can be found in the literature: Chem.Commun., 2013, 49, 9449-9451. Put phthalic acid and 1.2g acetic acid in 16mL N, N-dimethylformamide, put them into a 200mL high-temperature autoclave after ultrasonic dispersion, and keep the temperature at 120°C for 24 hours. After the reaction, the reactants were cooled to room temperature and centrifuged The solid is separated, washed with N,N-dimethylformamide and chloroform for 4 to 6 times, centrifuged to separate the solid, and dried in vacuum at 50°C for 12 hours to obtain the obtained product.
[0058] Put 0.6g of the above-prepared MOFs into 20mL of chloroform, add 2.45g of methacrylic anhydride and 279.5mg of acid-binding agent triethylamine, mix well, stir and react at 60°C for 48 hours, separate the solid by centrifugation, and After washing with chloroform three times and drying in vacuum at 50 °C for 8 hours, vinyl-...
Embodiment 1
[0062] A preparation method of cage polysilsesquioxane / metal-2-aminoterephthalic acid organic framework hybrid material (POSS / MOFs), comprising steps:
[0063] Octavinyl cage polysilsesquioxane (201.0 mg) and initiator azobisisobutyronitrile (3.0 mg) were dissolved in 20 mL of anhydrous THF, and the above-prepared vinyl functionalized MOFs (metal ion for Zr 4+ ion cluster) (202.3 mg) and ultrasonically dispersed for 30 minutes, polymerized at 60°C for 8 hours under a nitrogen atmosphere, stopped the reaction, collected the solid product, washed three times with tetrahydrofuran, and dried at 70°C for 12 hours to obtain Take –NHCOCH(CH 3 )(CH 2 ) 3 – POSS / MOFs hybrid materials that connect bridges between POSS units and MOFs units, with a yield of 95.7%.
[0064] image 3 For the XRD spectrogram of the POSS / MOFs hybrid material prepared in this embodiment, it can be seen from the figure that the crystal structure diffraction peak of cage-free polysilsesquioxane in the prepa...
Embodiment 2
[0066] A preparation method of cage polysilsesquioxane / metal-2-aminoterephthalic acid organic framework hybrid material (POSS / MOFs), comprising steps:
[0067] Octavinyl cage polysilsesquioxane (211.7 mg) and initiator azobisisobutyronitrile (3.8 mg) were dissolved in 30 mL of anhydrous chloroform, and the vinyl-functionalized MOFs prepared above were added ( Metal ion is Zr 4+ ion cluster) (127.4 mg) and ultrasonically dispersed for 30 minutes, polymerized at 65°C under argon for 10 hours, collected the solid product after stopping the reaction, washed 3 times with chloroform, and then dried at 70°C for 12 hours , obtained with –NHCOCH(CH 3 )(CH 2 ) 3 – POSS / MOFs hybrid materials that connect bridges between POSS units and MOFs units, with a yield of 96.2%.
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