A kind of preparation method of binuclear manganese substituted silicon tungsten oxygen cluster catalyst
A manganese substitution and catalyst technology, which is applied in the field of preparation of binuclear manganese substitution silicotungsten oxygen cluster catalysts, can solve the problems of tedious TBzTD process and insufficient green oxidant, and achieve the effect of simple preparation method
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Embodiment 1
[0026] Example 1 Compound K 20 (H 2 O) 28 mn 2 (H 2 O) 4 Si 4 W 40 o 140 The preparation, its synthetic steps are as follows:
[0027] Add K successively to a clean beaker 6 Na 2 [SiW 11 o 39 ]∙13H 2 O (1g) and 10 mL of distilled water were stirred for 15 min, manganese chloride (0.1g) was added, potassium acetate (0.5g) was added, and acetic acid was used to adjust the pH value to 3, and the reaction was carried out for 7 hours. After the reaction was completed, it was cooled to room temperature, filtered, and the filtrate was slowly evaporated at room temperature, and block single crystals were obtained after 5-7 days. The yield is about 26%.
Embodiment 2
[0028] Example 2 Compound K 20 (H 2 O) 28 mn 2 (H 2 O) 4 Si 4 W 40 o 140 The preparation, its synthetic steps are as follows:
[0029] Add K successively to a clean beaker 6 Na 2 [SiW 11 o 39 ]∙13H 2 O (1g) and 10 mL of distilled water, stirred for 15 min, added manganese chloride (0.1g), then potassium acetate (0.5g), using acetic acid, adjusted the pH value to 4, reacted for 7h, after the reaction was completed, cooled to room temperature, filtered, and the filtrate was slowly evaporated at room temperature, and block single crystals were obtained after 5-7 days. The yield is about 37%.
Embodiment 3
[0030] Example 3 Compound K 20 (H 2 O) 28 mn 2 (H 2 O) 4 Si 4 W 40 o 140 The preparation, its synthetic steps are as follows:
[0031] Add K successively to a clean beaker 6 Na 2 [SiW 11 o 39 ]∙13H 2 O (1g) and 10 mL of distilled water, stir for 15 min, add manganese acetate (0.2g), then add potassium acetate (0.5g), use acetic acid, adjust the pH value to 4, react for 7h, after the reaction is completed, cool to room temperature , filtered, and the filtrate was slowly evaporated at room temperature, and block single crystals were obtained after 5-7 days. The yield is about 49%.
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