Fluorine-contained T-shaped zeolite molecular sieve and preparation method thereof
A technology of zeolite molecular sieve and fluorine source, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of no fluorine-containing T-type zeolite molecular sieve, no F element found, and direct introduction of fluorine atoms, etc., to achieve simple and easy to repeat the preparation process, The method is simple and easy to operate, reducing the effect of subsequent processing
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Embodiment 1
[0033] Embodiment 1: Preparation of fluorine-containing T-type zeolite molecular sieve
[0034] Choose aluminum hydroxide as the aluminum source, silica sol as the silicon source, and ammonium fluoride as the fluorine source. Under stirring, add the aluminum source to the lye of potassium hydroxide, heat to dissolve, and then slowly add the silicon source and the fluorine source In the lye, the addition rate of silica sol is controlled at 0.5-2ml / min, and the formed SiO 2 -K 2 O-Al 2 o 3 -MF-H 2 O system, the sol ratio is expressed as the molar ratio of each substance: SiO 2 / Al 2 o 3 =20,H 2 O / SiO 2 =20,K 2 O / SiO 2 =0.35, MF / SiO 2 = 0.1, after the sol was stirred and aged at 60°C for 24 hours, 0.5wt% nanometer molecular sieve seeds were added; the sol was loaded into a reactor, hydrothermally synthesized at a synthesis temperature of 100°C for 3 days, centrifuged, washed and dried to obtain fluorine-containing T-type zeolite molecular sieve.
[0035] The synthesi...
Embodiment 2
[0037] Embodiment 2: Preparation of fluorine-containing T-type zeolite molecular sieve
[0038] The synthesis process was as described in Example 1, except that the synthesis temperature was increased to 160° C. and the synthesis time was shortened to 1 day. The reaction product was washed by centrifugation until the pH value was neutral, and dried at 110° C. for 12 hours. The synthesized molecular sieves were characterized by X-ray diffraction as pure T-type zeolite molecular sieve crystals. 19 Characterization of F and SiF by solid-state NMR technology x 4-x The form exists, indicating that F is completely incorporated into the crystal framework.
Embodiment 3
[0039] Embodiment 3: Preparation of fluorine-containing T-type zeolite molecular sieve
[0040] The synthesis process is as described in Example 1, except that ammonium fluoride is changed into sodium fluoride. The reaction product was cleaned by centrifugation until the pH value was neutral, and dried at 110° C. for 12 hours. The synthesized molecular sieves were characterized by X-ray diffraction as pure T-type zeolite molecular sieve crystals. 19 Characterization of F and SiF by solid-state NMR technology x 4-x The form exists, indicating that F is completely incorporated into the crystal framework. Elemental analysis showed that the F / Si molar ratio in the crystals decreased to 0.12%.
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