Gold cluster catalyst and method for producing same
A manufacturing method, technology of gold clusters, applied in catalyst activation/preparation, organic chemistry methods, chemical instruments and methods, etc., to achieve high selectivity
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Embodiment 1
[0114] [Example 1] Preparation of a gold cluster catalyst with 11 gold atoms
[0115] (Synthesis of Chloro(triphenylphosphine)Au(I))
[0116] 1 g of chloroauric acid tetrahydrate was added to 35 mL of ethanol under a nitrogen atmosphere, and stirred and dissolved to obtain a chloroauric acid solution. 50 ml of an ethanol solution in which 1.364 g of triphenylphosphine was dissolved was added to the above-mentioned chloroauric acid solution under a nitrogen atmosphere to perform a reaction. The reaction solution changed from yellow to white, and a white precipitate was formed. The precipitate was dissolved in 5ml of dichloromethane, 120ml of pentane was slowly added, and it was stored overnight in a refrigerator to precipitate a white substance, which was filtered by suction and vacuum-dried to obtain the product (chloro(triphenylene) base phosphine) Au(I)).
[0117] (Au 11 Synthesis of gold cluster compounds)
[0118] 0.25 g of the obtained chloro(triphenylphosphine)Au(I)...
Embodiment 2
[0143] [Example 2] Preparation of a gold cluster catalyst with 55 gold atoms
[0144] A gold cluster catalyst was obtained in the same manner as in Example 1, except that Au clusters were prepared as follows. Phosphine protected Au 55 The electron micrographs of the clusters are shown in Figure 7 , the histogram representing the gold cluster size is shown in Figure 8 .
[0145] (Au 55 cluster synthesis)
[0146] Chloro(triphenylphosphine)Au(I) (0.25 g) prepared in the same manner as in Example 1 was added to 20 ml of benzene under a nitrogen atmosphere, and stirred and dissolved. Next, borane-tetrahydrofuran complex (THF) (BH 3 -THF complex) solution 3ml, and stirred to obtain the product. The product was added to 5 ml of a dichloromethane solution, filtered and dried. Slowly add pentane 120ml in this product, filter, dry, thereby obtain final product (Au 55 clusters).
Embodiment 3
[0147] [Example 3] Preparation of a gold cluster catalyst with 101 gold atoms
[0148] A gold cluster catalyst was obtained in the same manner as in Example 1, except that Au clusters were prepared as follows. Phosphine protected Au 101 The electron micrographs of the clusters are shown in Figure 9 , the histogram representing the gold cluster size is shown in Figure 10 .
[0149] (Au 101 cluster synthesis)
[0150] 50 ml of distilled water (a solution) in which chloroauric acid (2.54 mmol) was dissolved and 65 ml of toluene (b solution) in which tetraoctylammonium bromide (TOAB) (2.93 mmol) was dissolved were prepared. The prepared a solution and b solution were mixed under a nitrogen atmosphere for 30 minutes to perform a reaction. Since the gold salt generated by the reaction migrated from the water layer to the toluene layer, water was removed from this solution with a 50 ml syringe, and vigorously stirred at room temperature. After 30 minutes, triphenylphosphine ...
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