Preparation method for precious-metal-containing titanium silicalite material
A titanium silicalite and precious metal technology, which is applied in the field of preparation of precious metal-containing titanium silicalite materials, can solve problems such as the need to be improved in activity and activity stability, and achieve good catalytic activity stability, good dispersibility and stability, and synergistic effect. improved effect
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Embodiment 1
[0034] Add tetrapropylammonium hydroxide aqueous solution containing palladium acetate and Tween 80 into tetraethyl orthosilicate and tetrabutyl titanate mixture and stir well, wherein the molar composition is silicon source: titanium source: protective agent: organic Alkali: palladium source: water = 100: 0.1: 0.2: 0.02: 0.1: 600, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then add hydrazine hydrate equimolar to the above-mentioned palladium source, then transfer the result to a stainless steel sealed reactor for hydrothermal treatment at a temperature of 170°C and autogenous pressure for 36 hours, take out the result and dry it naturally at room temperature until the water content is less than 10 % by weight, washed with water, filtered, dried at 150°C, and calcined at 550°C for 3 hours to obtain noble metal-containing titanium-silicon material A. The X-ray diffraction spectrum of the material has the spectrum ...
Embodiment 2
[0036] Add the tetrapropylammonium hydroxide aqueous solution containing palladium ammonium chloride and Span 60 into the mixed solution of tetraethyl orthosilicate and tetrabutyl titanate and stir well, wherein the molar composition is silicon source: titanium source: protective agent : organic base: palladium source: water = 100: 1.0: 0.8: 1.0: 0.2: 1500, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then add 2 times the hydrazine hydrochloride with the above-mentioned palladium source (mole), then transfer the result to a stainless steel sealed reaction vessel and treat it for 48 hours at a temperature of 120°C and autogenous pressure, and take out the result and dry it naturally at room temperature to the water content Less than 10% by weight, washed with water, filtered, dried at 150°C, and calcined at 550°C for 3 hours to obtain the noble metal-containing titanium-silicon material B. The X-ray diffraction spec...
Embodiment 3
[0038] A mixed aqueous solution of tetrapropylammonium hydroxide and triethanolamine containing palladium nitrate and cyclodextrin was added to tetraethyl orthosilicate and TiCl 4 Stir and mix in the mixed solution, wherein the molar composition silicon source: titanium source: protective agent: organic base (the molar ratio of tetrapropyl ammonium hydroxide and triethanolamine is 1): palladium source: water=100: 0.03: 0.5: 0.05 :0.02:550, the silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then add hydrazine hydrate equimolar to the above-mentioned palladium source, then transfer the result to a stainless steel sealed reaction kettle for 36 hours at a temperature of 100°C and autogenous pressure, take out the result and let it dry naturally at room temperature until the water content is less than 10 % by weight, washed with water, filtered, dried at 150°C, and calcined at 550°C for 3 hours to obtain the noble metal-c...
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