Tin-silicon molecular sieve and preparation method thereof
A technology of tin-silicon molecular sieve and silicon molecular sieve, which is applied in the field of tin-silicon molecular sieve and its preparation
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[0029] In the preparation method of the present invention, the silicon molecular sieve can be MFI structure (such as S-1), MEL structure (such as S-2), BEA structure (such as Beta), MWW structure (such as MCM-22), di At least one of three-dimensional hexagonal structure (such as MCM-41, SBA-15), MOR structure (such as MOR), TUN structure (such as TUN) and silicon molecular sieves with other structures (such as ZSM-48, MCM-48). Preferably, the silicon molecular sieve is one or more of silicon molecular sieves with MFI structure, MEL structure and BEA structure, more preferably MFI structure silicon molecular sieves.
[0030] In the present invention, the silicon molecular sieve is commercially available or can be prepared, and the method for preparing the silicon molecular sieve is well known to those skilled in the art, and will not be repeated here.
[0031] In the present invention, the tin-silicon molecular sieve is prepared by introducing tin element in the gas-solid phase...
Embodiment 1
[0055] (1) At 25°C, mix the tin source and silicon molecular sieve in solid phase for 30 minutes to obtain a mixture of tin source and silicon molecular sieve;
[0056] (2) Add template solution to the mixture of tin source and silicon molecular sieve mentioned in step (1) (during this contact process, add water or not add water according to the need, if the feeding in step (1) can meet the feeding requirements of water , then no need to add water, if not satisfied, you can additionally add water when the mixture containing tetrapropylammonium hydroxide, tin chloride and silicon molecular sieve is stirred and contacted, the rest of the examples are similar, no need to repeat the description); wherein, guarantee The molar ratio of each material is: silicon source (silicon molecular sieve): alkali source templating agent (tetrapropyl ammonium hydroxide): tin source (crystalline tin tetrachloride): water=100:10:0.5:20, wherein, SiO 2 Tin source is calculated as tin element;
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Embodiment 2
[0073] (1) At 25°C, mix the tin source and silicon molecular sieve in solid phase for 60 minutes to obtain a mixture of tin source and silicon molecular sieve;
[0074] (2) Add template solution to the mixture of said tin source and silicon molecular sieve in step (1); wherein, ensure that the molar ratio of each material is: silicon source (silicon molecular sieve): alkali source template (tetrapropyl Ammonium hydroxide): tin source (crystalline tin tetrachloride): water=100:15:0.1:10, wherein the silicon source is SiO 2 Tin source is calculated as tin element;
[0075] (3) Transfer the above mixture into a stainless steel sealed reaction kettle, crystallize at 160°C and autogenous pressure for 120h, filter the resulting crystallized product, wash with water, and dry at 110°C for 120 minutes, then at 550°C Roasting at high temperature for 3 hours to obtain tin-silicon molecular sieves.
[0076] According to the XRF composition analysis, the mass percentage of Sn is 1.0; in ...
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