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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

Inactive Publication Date: 2015-05-13
李亚丰
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this type of catalyst has excellent catalytic activity, the separation of the catalyst limits the application of this type of catalyst
In addition, such materials can also be supported such as Al 2 o 3 , SiO 2 , ZrO 2 However, due to the wide distribution of pores in this type of material, the catalyst is easy to fall off under the action of solvents, so although there are many reports in the literature, there are few practical applications

Method used

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  • Heteropolyacid or heteropolyacid salt and microporous coordination polymer composite material and preparation method thereof
  • Heteropolyacid or heteropolyacid salt and microporous coordination polymer composite material and preparation method thereof
  • Heteropolyacid or heteropolyacid salt and microporous coordination polymer composite material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0047] Dissolve 150 mg of zirconium tetrachloride (0.644 mmol) into 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 half an hour of continuous stirring, 130 mg of terephthalic acid (0.787 mmol) was dissolved in this mixture, followed by 12.2 mg of Na 3 PMo 12 o 40 ·xH 2 O (0.00644 mmol). The mixture was microwaved at 140°C for 2 hours, taken out, centrifuged, washed, and dried at 120°C to obtain the product with a yield of 91%. The product has been subjected to X-ray powder diffraction ( figure 1 ), its diffraction peak position is the same as that of UIO-66 (ZrO(O 2 C-C 6 h 4 -CO 2 )) are consistent, indicating that the main body of the composite material is UIO-66, and the crystallinity is relatively high; Fourier transform infrared spectroscopy analysis ( figure 2 ), the infrared characteristic vibration peak is consistent with UIO-66, and there is also the infrared...

Embodiment 2

[0049] Dissolve 150 mg of zirconium tetrachloride (0.644 mmol) into 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-naphthalene dicarboxylic acid (0.72 mmol) was dissolved in this mixture, followed by 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, taken out, centrifuged, washed, and dried at 120°C to obtain the product with a yield of 89%. The product has been subjected to 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 relatively high; Fourier transform infrared spectroscopy analysis ( Figure 4 ), the infrared characteristic vibration peak is consistent with IRUIO-66, and there is als...

Embodiment 3

[0051] 131 mg of zirconyl sulfate (0.644 mmol) was dissolved under stirring into a mixed solvent of 3 ml of acetic acid (52.4 mmol) and 40 ml of N, N'-dimethylformamide (516 mmol) to obtain a clear solution, After continuous stirring for half an hour, 125 mg of 4,4'-biphenyldicarboxylic acid (0.51 mmol) was dissolved in this mixture, followed by 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, taken out, centrifuged, washed, and dried at 120°C to obtain the product with a yield of 85%. The product has been subjected to X-ray powder diffraction ( Figure 5 ), its diffraction peak position is the same as that of 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 relatively high; Fourier transform infrared spectroscopy analysis ( Figure 6 ), the infrared characteristic vibration peak is consistent with UIO-67, and there is also the infrar...

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Abstract

The invention relates to a heteropolyacid or heteropolyacid salt and microporous coordination polymer composite material and a preparation method thereof. The preparation method is characterized by comprising the following steps: a first step of dissolving zirconium salt in a mixed solvent of a modifier and a solvent to form a settled solution while stirring at the normal temperature and under the normal pressure; a step 2 of adding the settled solution obtained in the first step into an organic ligand until the settled solution is dissolved; a third step of adding heteropolyacid or heteropolyacid salt into the settled solution obtained in the second step to prepare a mixed solution and enabling the mixed solution to react to obtain the heteropolyacid or heteropolyacid salt and zirconium-based microporous coordination polymer composite material, wherein by calculating according to the added zirconium salt, the yield of the heteropolyacid or heteropolyacid salt and microporous coordination polymer composite material is 85-93 percent.

Description

technical field [0001] The patent of the present invention relates to the composite material of heteropolyacid or heteropolyacid salt and microporous coordination polymer and its preparation method. Background technique [0002] So far, more than 10,000 kinds of coordination polymers have been synthesized, some of which have been widely accepted due to their very high thermal stability and chemical stability (organic solvents, water, acid or alkali, air, etc.). Of concern, these coordination polymers include, for example: HKUST-1, MIL-100, MIL-101, ZIF-8 and UIO-66, etc. where by Zr 6 o 4 (OH) 4 (CO 2 ) 12 UIO-66, 67, and 68 composed of clusters and UIO-66, 67, and 68 with functional groups have thermal stability close to 500°C, as well as acid and alkali resistance. In terms of structure, take UIO-66 as an example. Its structure has a very high symmetry and a cubic Fm-3m space group. The structure contains both tetrahedral cavities and octahedral cavities. All molecu...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/18B01J31/16
Inventor 李亚峰张李梅
Owner 李亚丰
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