A kind of preparation method of two-dimensional nanoporous structure pd-cof material
A porous structure, two-dimensional nanotechnology, applied in the field of photocatalytic materials, can solve the problems of low crystallinity, slow multi-electron diffusion-control, etc., and achieve excellent adsorption performance, good chemical stability, and mild reaction conditions.
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[0039] A preparation method of a two-dimensional nanoporous structure Pd-COF material, comprising the following steps:
[0040] Step 1, using 4,6-diaminoresorcinol dihydrochloride and 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine as raw materials, using gradient thermal polycondensation method Preparation of organic framework materials COF, such as figure 1 As shown, specifically:
[0041] Step 1.1: Weigh the synthetic raw materials 4,6-diaminoresorcinol dihydrochloride, 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine, of which 4,6 - The molar ratio of diaminoresorcinol dihydrochloride to 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine is 1.2:1 to 1.5:1.
[0042] Step 1.2: Stir the 4,6-diaminoresorcinol dihydrochloride weighed in step 1.1 in polyphosphoric acid, wherein 4,6-diaminoresorcinol dihydrochloride and polyphosphoric acid The molar volume ratio is 10-15mmol / L, and the dehydrochlorination process needs to be stirred at a temperature of 65-80°C for 8-10 hours under the protection...
Embodiment 1
[0057] Step 1: Using 4,6-diaminoresorcinol dihydrochloride and 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine as raw materials, adopt gradient thermal polycondensation method Prepare the organic framework material COF, specifically:
[0058] Step 1.1: Weigh the synthetic raw materials 4,6-diaminoresorcinol dihydrochloride, 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine, of which 4,6 - The ratio of the amount of substances of diaminoresorcinol dihydrochloride and 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine is 1.2:1,4,6- The amount of substance of diaminoresorcinol dihydrochloride is 1.7mmol, and the amount of substance of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine is 1.13mmol;
[0059] Step 1.2: Stir the 4,6-diaminoresorcinol dihydrochloride weighed in step 1.1 in polyphosphoric acid at 70°C for 8 hours under the protection of nitrogen, wherein, 4,6-diaminoresorcinol dihydrochloride The molar volume ratio of hydrochloride to polyphosphoric acid is 10mmol / L;
[0060] Step 1.3: Add the...
Embodiment 2
[0077] Step 1: Using 4,6-diaminoresorcinol dihydrochloride and 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine as raw materials, adopt gradient thermal polycondensation method Prepare the organic framework material COF, specifically:
[0078] Step 1.1: Weigh the synthetic raw materials 4,6-diaminoresorcinol dihydrochloride, 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine, of which 4,6 -Diaminoresorcinol dihydrochloride and 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine in a molar ratio of 1.35:1,4,6-diaminom-benzene The amount of substance of diphenol dihydrochloride was 1.9125 mmol, the amount of substance of 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine was 1.42 mmol;
[0079] Step 1.2: Stir the 4,6-diaminoresorcinol dihydrochloride weighed in step 1.1 in polyphosphoric acid at 65°C for 9 hours, wherein, 4,6-diaminoresorcinol dihydrochloride The molar volume ratio with polyphosphoric acid is 12mmol / L;
[0080]Step 1.3: Add the 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine weighed in step 1.1...
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