Titanium silicon molecular sieve, synthetic method and applications thereof, and cyclic ketone oxidation method
A titanium-silicon molecular sieve and synthesis method technology, applied in molecular sieve compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of small grain size, insufficient reactivity, complex process, etc., and achieve improved selectivity and good catalytic activity. The effect of stability and high utilization rate
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[0032] In the present invention, as long as the titanium-silicon molecular sieve has the aforementioned characteristics, the purpose of the present invention can be achieved, and its synthesis method can be various, as long as the titanium-silicon molecular sieve with the aforementioned characteristics can be synthesized. For the present invention, the titanium-silicon molecular sieve is preferably Silicon molecular sieves are synthesized as follows, the method comprising:
[0033] In the presence of a water-containing solvent, the silicon source, the titanium source and the alkali source are mixed and then hydrothermally crystallized under airtight conditions to recover titanium-silicon molecular sieves; wherein, the hydrothermal crystallization goes through stage (1) and stage ( 2) and stage (3), stage (1) is crystallized at 80-120°C, stage (2) is heated to 180-220°C for crystallization, and stage (3) is cooled to 140-180°C for crystallization.
[0034]According to a preferr...
Embodiment approach
[0037] According to a preferred embodiment of the present invention, silicon source: titanium source: alkali source: the molar ratio of water is 100: (0.5-5): (10-50): (500-5000), preferably 100: (2 -4): (15-35): (1000-3000) Among them, the silicon source is SiO 2 Meter, titanium source as TiO 2 In terms of alkali source in N or OH - count.
[0038] According to the method of the present invention, the aqueous solvent basically contains water, and a co-solvent may also be added as required. In an embodiment of the present invention, the aqueous solvent is water.
[0039] In the present invention, the silicon source may be an inorganic silicon source and / or an organic silicon source.
[0040] Specifically, the organosilicon source can be, for example, one or more selected from the silicon-containing compounds shown in formula I,
[0041]
[0042] In formula I, R 1 , R 2 , R 3 and R 4 Each is C 1 -C 4 Alkyl groups, including C 1 -C 4 straight-chain alkyl and C 3 ...
Embodiment 1
[0090] Add 20 grams of silicon source tetraethyl orthosilicate to tetrapropyl ammonium hydroxide aqueous solution and stir to mix evenly, then add tetrabutyl titanate and mix evenly to obtain the molar composition: silicon source: titanium source: alkali source: Water = 100:2:15:1000 mixture. Put the mixture in a sealed stainless steel reaction kettle, raise the temperature of the kettle from room temperature to 100°C at a heating rate of 2°C / min and perform hydrothermal treatment at this temperature for 24 hours, and then raise the temperature of the kettle to 190°C at a heating rate of 15°C / min And hydrothermal treatment at this temperature for 6 hours; then reduce the temperature of the kettle to 170 °C at a cooling rate of 10 °C / min and hydrothermal treatment at this temperature for 48 hours, and finally cool down to room temperature and release the pressure, the product in the reactor is filtered, Washing, drying and calcination at 550° C. for 5 hours to obtain titanium s...
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