Preparation method of hollow single crystal Beta molecular sieve
A molecular sieve and single crystal technology, applied in the field of catalytic chemistry, can solve the problems of cumbersome preparation process, harsh conditions and restrictions on industrial production of multi-stage porous or hollow Beta molecular sieves, and achieve high crystallinity, large specific surface area and pore volume, and simple The effect of the preparation method
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Embodiment 1
[0036] Under stirring conditions, 5.3g of white carbon black (95.0wt.% SiO 2 , 5.0wt.%H 2 O), 0.4g sodium aluminate (49.0wt.%Al 2 o 3 , 38.0 wt.% Na 2 O, 13.0 wt.% H 2O), 0.13g sodium hydroxide (96.0wt.% NaOH), 22.3g tetraethylammonium hydroxide aqueous solution (TEAOH, purity ≥ 35wt.%), 25g N-methyl-2 pyrrolidone (NMP, ≥ 99wt.% ), 9g of deionized water were added to the reactor in a certain order. The molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =43.5,Na 2 O / SiO 2 = 0.048, TEA + / SiO 2 =0.636, NMP / SiO 2 =3.0,H 2 O / SiO 2 =16. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (30 rpm) at 140°C for 60h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 80°C to obtain molecular sieve powder.
[0037] figure 1 It is the powder X-ray diffraction pattern of the obtained molecular sieve powd...
Embodiment 2
[0042] Under stirring condition, 19.5g water glass (26wt.%SiO 2 , 8.2 wt.% Na 2 O, 65.8 wt.% H 2 O), 1.29g aluminum sulfate (≥99wt.%), 1.9g potassium hydroxide (≥99wt.%), 25g tetraethylammonium chloride aqueous solution (TEACl, purity ≥35wt.%), 25g N-methyl- 2 Pyrrolidone is added to the reaction kettle in a certain order. The molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =43.5, K 2 O / SiO 2 = 0.2, TEA + / SiO 2 =0.636, NMP / SiO 2 =3.0,H 2 O / SiO 2 =16. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (100 rpm) at 100°C for 240h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 80°C to obtain molecular sieve powder.
[0043] The XRD spectrum pattern of gained Beta product and figure 1 Similarly, transmission electron microscopy (TEM) pictures show that it is a hollow single crystal structur...
Embodiment 3
[0045] Under stirring conditions, 17.4g ethyl orthosilicate (≥99wt.%), 2.0g aluminum chloride (≥99wt.%), 2.7g sodium hydroxide, 3.5g tetraethylammonium hydroxide aqueous solution, 43g N -Ethyl-2-pyrrolidone and 9g of deionized water were added to the reaction kettle in a certain order. The molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =20,Na 2 O / SiO 2 = 0.4, TEA + / SiO 2 =0.1, NEP / SiO 2 =6.0,H 2 O / SiO 2 =16. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (80 rpm) at 100°C for 200h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 80°C to obtain molecular sieve powder.
[0046] The XRD spectrum pattern of gained Beta product and figure 1 Similarly, transmission electron microscopy (TEM) pictures show that it is a hollow single crystal structure with a particle size of about 312nm, N 2 Th...
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