Preparation method of titanium silicalite molecular sieve catalyst for improving content of tetravalent titanium in skeleton structure and catalyst
A titanium-silicon molecular sieve and framework structure technology, which can be used in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., and can solve problems such as low tetravalent titanium content
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Embodiment 1
[0037] Add 0.28g of citric acid monohydrate to 24.98g of 25% tetrapropylammonium hydroxide and 15.88g of H 2 O solution, stirred for 0.5 hours to dissolve it. 2.18 g of tetrabutyl titanate was added dropwise to the above solution, and stirred at room temperature for 0.5 hours. Then, 40 g of tetraethyl orthosilicate was added dropwise into the above clear solution, and stirred at room temperature for 1 hour. The obtained jelly was transferred to a tank reactor with a polytetrafluoroethylene liner of 100 ml, and crystallized at 170° C. for 24 hours. The product was suction filtered, dried, and calcined in a muffle furnace at 550°C for 2 hours to obtain a molecular sieve product. The material ratio (molar ratio) of reactant is:
[0038] SiO 2 / TiO 2 =30
[0039] Citric acid / SiO 2 =0.0075
[0040] TPAOH / SiO 2 =0.16
[0041] h 2 O / SiO 2 =10
[0042] The calcined samples were measured, and the UV-visible light absorption intensity data are shown in Table 1.
[0043] Ta...
Embodiment 2
[0047]Add 0.70g oxalic acid to 24.98g tetrapropylammonium hydroxide, 1.02g tetrapropylammonium bromide and 33.18gH 2 O solution, stirred for 0.5 hours to dissolve it. 6.54 g of tetrabutyl titanate was added dropwise to the above solution, and stirred at room temperature for 0.5 hours. Then 38.46 g of 30% silica sol was added dropwise to the above clear solution, and stirred at room temperature for 1 hour. The obtained jelly was transferred to a tank reactor with a polytetrafluoroethylene liner of 100 ml, and crystallized at 172° C. for 48 hours. The product was suction filtered, dried, and calcined in a muffle furnace at 550°C for 2 hours to obtain a molecular sieve product. The material ratio (molar ratio) of reactant is:
[0048] SiO 2 / TiO 2 =10
[0049] Oxalic acid / SiO 2 =0.007
[0050] TPAOH / SiO 2 =0.16
[0051] TPABr / SiO 2 =0.02
[0052] h 2 O / SiO 2 =15
[0053] The calcined samples were measured, and the UV-visible light absorption intensity data are show...
Embodiment 3
[0058] Add 0.57g tartaric acid to 7.67g 25% tetrapropylammonium bromide, 5.80g 35% tetraethylammonium hydroxide and 62.31gH 2 O solution, stirred for 0.5 hours to dissolve it. 4.36 g of tetraethyl titanate was added dropwise to the above solution, and stirred at room temperature for 0.5 hour. Then 11.53 g of solid silicon oxide was added dropwise to the above clear solution, and stirred at room temperature for 1 hour. The obtained jelly was transferred to a tank reactor and crystallized at 165° C. for 72 hours. The product was suction filtered, dried, and calcined in a muffle furnace at 550°C for 4 hours to obtain a molecular sieve product. The material ratio (molar ratio) of reactant is:
[0059] SiO 2 / TiO 2 =15
[0060] Tartaric acid / SiO 2 =0.02
[0061] TPABr / SiO 2 =0.15
[0062] TEAOH / SiO 2 =0.20
[0063] h 2 O / SiO 2 =18
[0064] The calcined samples were measured, and the UV-visible light absorption intensity data are shown in Table 3.
[0065] table 3
...
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