Pyramid-shaped polyoxometallate-polyhedral oligomeric silsesquioxane hybrid molecule as well as preparation method and application thereof
A polyoxometalate, silsesquioxane technology, applied in chemical instruments and methods, polycrystalline material growth, crystal growth and other directions, can solve problems such as poor solubility and difficult processing
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Embodiment 1
[0040] Taking the synthesis of pyramidal polyoxometalate-cage silsesquioxane hybrid molecules as an example, the synthesis route is shown in Figure 1, and the specific implementation steps are as follows:
[0041] Step 1, 2 t Synthesis of Bu-Fmoc
[0042] 2 t Bu-NH 2 (4.16g, 10.0mmol) was dissolved in about 100mL THF, Fmoc-OSu (3.71g, 11.0mmol) was added, and stirred at room temperature for 24h. Spot plate monitoring, until the reaction is complete, spin off the solvent. Purified by silica gel column chromatography (200-300 mesh), the eluent was petroleum ether:ethyl acetate=3:1 (volume ratio), and dried to obtain 6.25g of white solid 2 t Bu-Fmoc (yield: 98%).
[0043] The synthesis of step 2,2POSS-DL-Fmoc
[0044] Select the 2 obtained in step 1) t Bu-Fmoc (2.62g, 5.0mmol), dissolved in 100mL of anhydrous formic acid, stirred at room temperature for 24h, after the reaction was complete, the formic acid was removed by spin. Subsequently, about 30 mL of toluene was adde...
Embodiment 2
[0067] Preparation of Colloidal Crystals of Pyramidal Caged Silsesquioxane-Polymetallic Oxygen Cluster Hybrid Molecules.
[0068] 1) Preparation of precursor solution:
[0069] Using the 4POSS-DL-POM hybrid molecule as the base material, weigh 6 mg, add 600 μL acetone solvent and 400 μL n-decane solvent, the total volume of the obtained precursor solution is 1.0 mL, and the sample concentration is 6.0 mg / mL;
[0070] 2) Preparation of colloidal crystals:
[0071] Put the above precursor solution in a 2.0mL sample bottle, and volatilize in the open at 25°C for 12 hours, and the solution obtained at this time is a nanoparticle suspension solution. The solution was dropped onto the carbon film, evaporated slowly, and dried in vacuum to obtain colloidal crystals.
[0072] The present invention focuses on the assembly process and structural changes. In its acetone and n-decane mixed solution, the opening is placed, and the acetone volatilizes, and it slowly assembles. It can be o...
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