CHA-type silicon-aluminum molecular sieves, and preparation methods and applications thereof
A silicon-aluminum molecular sieve and silicon-aluminum ratio technology, which is used in separation methods, molecular sieve catalysts, chemical instruments and methods to achieve uniform distribution, cost savings, and controllable grain size.
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[0067] As mentioned above, the present invention discloses a method for preparing the above-mentioned CHA-type silica-alumina molecular sieve, which comprises the following steps:
[0068] 1) Prepare sol: mix template agent, alkali and water, add aluminum source and silicon source, stir evenly between 25-45°C;
[0069] 2) Get the sol of step 1), join in the autoclave, add 0.1-5wt% weight (relative to SiO in the silicon source 2 weight) seed crystals, stirred, and crystallized at 165-190°C for 10-30 hours, wherein the stirring speed was 80-240rpm;
[0070] Wherein, the alkali is potassium hydroxide (KOH).
[0071] 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.
[0072] In the present invention, the aluminum source is selected from one or more of aluminum nitrate, aluminum hydroxide, pseudoboehmite, aluminum oxide, aluminum powder and aluminum sulfat...
Embodiment 1
[0085] Embodiment 1 (preparation CHA type silica-alumina molecular sieve)
[0086] Prepare CHA-type silica-alumina molecular sieves through the following steps:
[0087] 1) Colloidal preparation: add template agent (75.92g, 23.25%, 0.084mol), KOH (104.0g, 91.17%, 1.69mol) in 800g of water to prepare the solution, and aluminum sulfate (46.95g, 0.070 mol) was dissolved in 270g of water, and after stirring for half an hour, silica sol (498.42g, 30.00%, 2.49mol) was added, and a uniform translucent colloid was obtained after stirring at 35°C for half an hour.
[0088] The molecular formula of the templating agent is (R 1 -N + (R 2 ) 3 ) m A m- , where R 1 for adamantane, R 2 They are the same as methyl, m is equal to 1, and A is hydroxide, which is obtained from purchase.
[0089] 2) Transfer the colloid in step 1) to a 2L autoclave, add 2.5g of seed crystals, crystallize at 180°C for 10 hours under stirring at 120rpm, and filter to obtain the crude product of the CHA-typ...
Embodiment 2
[0099] Embodiment 2 (preparation of CHA type silica-alumina molecular sieve)
[0100] Prepare CHA-type silica-alumina molecular sieves through the following steps:
[0101] 1) Colloidal preparation: add template agent (176.73g, 23.25%, 0.20mol) and KOH (47.76g, 91.17%, 0.78mol) into a beaker to prepare a solution prepared by dissolving 760g of water, and then add aluminum sulfate (43.33 g, 0.065mol) was dissolved in 250g water to prepare the solution, after stirring for half an hour, silica sol (546.77g, 30.00%, 2.73mol) was added, and a uniform translucent colloid was obtained after stirring at 35°C for half an hour.
[0102] The molecular formula of the templating agent is (R 1 -N + (R 2 ) 3 ) m A m- , where R 1 for adamantane, R 2 They are the same as methyl, m is equal to 1, and A is hydroxide, which is obtained from purchase.
[0103] 2) Transfer the colloid in step 1) to a 2L autoclave, add 3.0g of seed crystals, crystallize at 180°C for 10 hours under stirring ...
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