cha type silicon aluminum phosphorus molecular sieve and its preparation method and application
A silicon-aluminum-phosphorus molecular sieve and silicon source technology, applied in separation methods, molecular sieve catalysts, chemical instruments and methods, etc., to achieve uniform distribution, controllable grain size, and cost-saving effects
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[0058] As mentioned above, the present invention discloses a preparation method of the above-mentioned CHA type silicon aluminum phosphorus molecular sieve, which comprises the following steps:
[0059] 1) Compounding sol: After adding silicon source, aluminum source and water to the mixed template agent, add phosphoric acid and stir evenly between 25-45°C;
[0060] 2) Get the sol of step 1), add 0.1-5wt% weight (relative to SiO in the silicon source 2 weight) seed crystals were added into the autoclave, stirred, and crystallized at 165-200° C. for 10-48 hours, wherein the stirring speed was 80-240 rpm.
[0061] In the present invention, the silicon source is selected from inorganic silicon. Preferably, it is silica sol containing silica or solid silica gel for column chromatography.
[0062] In the present invention, the aluminum source is selected from one or more of aluminum hydroxide, pseudoboehmite, aluminum oxide and aluminum powder.
[0063] In the present invention,...
Embodiment 1
[0073] The CHA type silicon aluminum phosphorus molecular sieve is prepared by the following steps:
[0074] 1) Colloidal sol: add silica sol (76.20g, 30%, 0.38 mol), after stirring for half an hour, add water (990 grams, 54.99 moles), and after stirring for half an hour, pseudo-boehmite (109.8g, 76.5%, 0.83mol), add phosphoric acid (219.60g, 85%, 1.91mol), Stir at 35°C for half an hour to obtain a homogeneous translucent colloid.
[0075] 2) Transfer the colloid in step 1) to a 2L autoclave, add 1.00g of seed crystals, crystallize at 180°C for 20 hours under stirring at 120rpm, and filter to obtain the crude product of the CHA-type silicon-aluminum-phosphorus molecular sieve (denoted as molecular sieve X).
[0076] Post-processing is performed as follows:
[0077] i) washing the above-mentioned molecular sieve X with water,
[0078] ii) calcining the product of step i) at 600° C. to obtain the final acidic CHA-type silicon-aluminum-phosphorus molecular sieve (referred to ...
Embodiment 2
[0082] The CHA type silicon aluminum phosphorus molecular sieve is prepared by the following steps:
[0083] 1) Colloidal sol: add triethylamine (278.94g, 99%, 2.67 moles) and adamantane ammonium (adamantane ammonium: R 1 -N + (R 2 ) 3 ) m A m- , where R 1 is adamantane, R 2 The same is methyl, A is hydroxide, m is equal to 186.43g, 23.25%, 0.096 moles), add silica sol (61.23g, 30%, 0.31 moles) to the two-component template agent, stir for half an hour, add water (1080 grams, 60.00 moles), add pseudo-boehmite (128.49g, 76.5%, 0.96 moles) and stir for half an hour, add phosphoric acid (241.36g, 85%, 2.10 moles), and stir for half an hour at 35°C to obtain a uniform half Transparent colloid.
[0084] 2) Transfer the colloid in step 1) to a 2L autoclave, add 0.80g of seed crystals, crystallize at 180°C for 15 hours under stirring at 120rpm, and filter to obtain the crude product of the CHA-type silicon-aluminum-phosphorus molecular sieve (denoted as molecular sieve Y). ...
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