Heteropolyacid or heteropolyacid salt and microporous coordination polymer composite material and preparation method thereof
A technology of coordination polymers and heteropoly acid salts, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, chemical/physical processes, etc. Problems such as few practical applications
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[0046] Example 1
[0047] 150 mg of zirconium tetrachloride (0.644 mmol) was dissolved in a mixed solvent of 5 ml of acetic acid (87.4 mmol) and 50 ml of N,N'-dimethylformamide (645 mmol) under stirring to obtain a clear solution After stirring continuously for half an hour, 130 mg terephthalic acid (0.787 mmol) was dissolved in the mixture, and then 12.2 mg Na 3 PMo 12 O 40 ·XH 2 O (0.00644 mmol). The mixture was microwaved at 140°C for 2 hours, centrifuged, washed, and dried at 120°C to obtain a product with a yield of 91%. The product has undergone X-ray powder diffraction ( figure 1 ), its diffraction peak position is the same as UIO-66(ZrO(O 2 C-C 6 H 4 -CO 2 )) consistent, indicating that the main body of the composite material is UIO-66, and the crystallinity is high; Fourier transform infrared spectroscopy ( figure 2 ), the infrared characteristic vibration peak is consistent with UIO-66, and there is also the infrared characteristic vibration peak of the guest molecule....
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[0048] Example 2
[0049] Dissolve 150 mg of zirconium tetrachloride (0.644 mmol) in a mixed solvent of 5 ml of acetic acid (87.4 mmol) and 40 ml of N,N'-dimethylformamide (516 mmol) under stirring to obtain a clear solution After stirring continuously for half an hour, 156 mg of 2,6-naphthalenedicarboxylic acid (0.72 mmol) was dissolved in the mixture, and then 167 mg of H 3 PMo 12 O 40 ·XH 2 O (0.092 mmol). The mixture was heated at 130°C for 36 hours, centrifuged, washed, and dried at 120°C to obtain a product with a yield of 89%. The product has undergone X-ray powder diffraction ( image 3 ), its diffraction peak position is the same as that of IRUIO-66(ZrO(O 2 C-C 10 H 6 -CO 2 )) consistent, indicating that the main body of the composite material is IRUIO-66, and the crystallinity is high; Fourier transform infrared spectroscopy ( Figure 4 ), the infrared characteristic vibration peak is consistent with IRUIO-66, in addition there is the infrared characteristic vibration p...
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[0050] Example 3
[0051] 131 mg of zirconyl sulfate (0.644 mmol) was dissolved in a mixed solvent of 3 ml of acetic acid (52.4 mmol) and 40 ml of N,N'-dimethylformamide (516 mmol) under stirring to obtain a clear solution. After stirring continuously for half an hour, 125 mg of 4,4'-biphthalic acid (0.51 mmol) was dissolved in the mixture, and then 59 mg of H 3 PMo 12 O 40 ·XH 2 O (0.0322 mmol). The mixture was heated at 130°C for 36 hours, centrifuged, washed, and dried at 120°C to obtain a product with a yield of 85%. The product has undergone X-ray powder diffraction ( Figure 5 ), its diffraction peak position is the same as UIO-67(ZrO(O 2 C-C 12 H 8 -CO 2 )) consistent, indicating that the main body of the composite material is UIO-67, and the crystallinity is high; Fourier transform infrared spectroscopy ( Image 6 ), the infrared characteristic vibration peak is consistent with UIO-67, in addition there is the infrared characteristic vibration peak of the guest molecule, ...
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