Small-grain multi-level porous ith structure silica-alumina molecular sieve and its preparation method and application
A silica-alumina molecular sieve and small-grain technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as difficulty in meeting industrial needs, poor repeatability of synthesis process, and poor selectivity of low-carbon olefins. Achieve the effects of improved service life, small diffusion resistance, and low carbon selectivity
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Embodiment 1
[0051] Under the condition of rapid stirring at 60°C, add 0.5mol / L dihydroxyhexanebisammonium R(OH) into the beaker 2 Aqueous solution 30mL (15mmol), then add 0.2g GeO 2 (1.95mmol), after dissolving, add 29.32g silica sol (n SiO2 =134.5mmol, in 27.5wt%) and 0.18g pseudo-boehmite (n Al2O3 =1.22mmol), continue to stir for 6 hours to obtain mixture A; in mixture A, add 4.0g (3.3mmol) polyoxyethylene sorbitan monolaurate (Tween 20) under stirring, the ITH structure silicon of 0.27g Alumina seeds and 1.63 g NH 4 F (44.1mmol), continue stirring at 60°C to form a uniform gel mixture, then transfer it to a stainless steel reaction kettle with polytetrafluoroethylene, filter it after crystallization for 3 days at 180°C, and filter at 120°C Dry overnight, roast at 540°C for 4 hours to obtain a small-grain ITH structure silica-alumina molecular sieve, then mix the obtained small-grain ITH structure silica-alumina molecular sieve with 0.2M NaOH aqueous solution at a mass volume ratio o...
Embodiment 2
[0061] Under the condition of rapid stirring at 70°C, add 1.0mol / L dihydroxyhexanebisammonium R(OH) into the beaker 2 The aqueous solution 300mL (300mmol), then add 4.5g (43mmol) GeO 2 , add 586.0g (n SiO2 =2816mmol, in 28.0wt%) tetraethyl orthosilicate and 1.8g pseudo-boehmite (n Al2O3 =7.9mmol), continue stirring for 20 hours to obtain mixture A; in mixture A, add 80.0g (62.0mmol) polyoxyethylene sorbitan monooleate (Tween 80), 2.7g of ITH structure under stirring Silica-alumina seed crystals and 29g NH 4 F (778mmol), continue stirring at 60°C to form a homogeneous gel mixture, then transfer it to a stainless steel reactor with polytetrafluoroethylene, filter it after crystallization for 3 days at 180°C, and dry at 120°C Overnight, roast at 540°C for 4 hours to obtain a small-grain ITH structure silica-alumina molecular sieve, and then mix the obtained small-grain ITH structure silica-alumina molecular sieve with 0.1M ammonia solution at a mass volume ratio of 1g:30mL, an...
Embodiment 3
[0063] Under the condition of rapid stirring at 50°C, add 1.0mol / L dihydroxyhexanebisammonium R(OH) into the beaker 2 The aqueous solution 400mL (400mmol), then add 4.5g (438.6mmol) GeO 2 , add 560g (n SiO2 =2688.0mmol, in 28.83wt%) water glass and 0.90g pseudo-boehmite (n Al2O3 =3.95mmol), continue to stir for 10 hours, obtain mixture A; In mixture A, add 80.6g (66mmol) polyoxyethylene sorbitan monolaurate (Tween 20) under stirring, the ITH structure silicon aluminum of 2.9g Zeolite seeds and 29 g NH 4 F (778mmol), continue to stir at 60°C to form a uniform gel mixture, transfer it to a stainless steel reaction kettle with polytetrafluoroethylene inside, filter it after crystallization for 3 days at 180°C, and dry at 120°C overnight , calcination at 540° C. for 4 hours to obtain a small-grain ITH structure silica-alumina molecular sieve, and then the obtained small-grain ITH structure silica-alumina molecular sieve was mixed with 0.3 M NaOH aqueous solution in a ratio of 1...
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