Method for controlling ts-1 molecular sieve crystal particle size and method for preparing small crystal ts-1 molecular sieve
A TS-1, crystal particle size technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of lack of adjustment of TS-1 molecular sieve crystal particle size
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preparation example 1
[0043] (1) Take 10g of ethyl orthosilicate, add 50g of water, add 0.5g of tetrabutyl titanate, add 1.3g of tetrapropylammonium bromide, stir evenly for 4 hours, pour it into a rotary self-pressure crystallization kettle at 150°C Crystallization for 24h;
[0044] (2) Filter the product obtained by crystallization in step (1), and then dry it in an oven at 100°C for 2h; place the dried solid in a muffle furnace, The heating rate was increased from room temperature (25°C) to 500°C, then roasted at a constant temperature of 500°C for 2 hours, and naturally cooled to room temperature to obtain TS-1 molecular sieve M1, as figure 1 As shown, the crystal grain size is 6×3×1 μm.
preparation example 2
[0046] (1) Take 10 g of solid silica gel, add 50 g of water, add 0.27 g of titanyl sulfate, add 6.8 g of tetrapropylammonium hydroxide, stir evenly for 4 hours, pour it into a rotary self-pressure crystallization kettle for crystallization at 180°C for 72 hours;
[0047] (2) Filter the product obtained by crystallization in step (1), and then dry it in an oven at 120°C for 4h; place the dried solid in a muffle furnace, The heating rate was raised from room temperature (25°C) to 600°C, then roasted at a constant temperature of 600°C for 4 hours, and naturally cooled to room temperature to obtain TS-1 molecular sieve M2 with a crystal particle size of 10×5×2 microns.
preparation example 3
[0049] (1) Take 10g of silica sol (SiO2 content 30%), add 50g of water, add 0.71g of isopropyl titanate, add 0.51g of tetrapropylammonium hydroxide, stir evenly for 4 hours, and pour it into a rotary self-pressure crystallization kettle Crystallization at 175°C for 48h;
[0050] (2) Filter the product obtained by crystallization in step (1), and then dry it in an oven at 110° C. for 3 h; place the dried solid in a muffle furnace, The heating rate was increased from room temperature (25°C) to 550°C, then roasted at a constant temperature of 550°C for 3 hours, and naturally cooled to room temperature to obtain TS-1 molecular sieve M3 with a crystal particle size of 5×2×0.5 microns.
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