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Hydrothermal synthesis method of nano Sn-Beta molecular sieve aggregate

A hydrothermal synthesis and molecular sieve technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of long crystallization time, large grain size, low tin content, etc., and achieve improved catalytic performance Effect

Active Publication Date: 2020-06-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to solve the problems of large grain size, long crystallization time, and low tin content in the traditional hydrothermal synthesis of Sn-Beta molecular sieves, it is proposed to use organosilane as an additive to synthesize nano-Sn-Beta molecular sieves by aerosol-assisted hydrothermal method

Method used

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  • Hydrothermal synthesis method of nano Sn-Beta molecular sieve aggregate
  • Hydrothermal synthesis method of nano Sn-Beta molecular sieve aggregate
  • Hydrothermal synthesis method of nano Sn-Beta molecular sieve aggregate

Examples

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Effect test

Embodiment 1

[0047] Synthesis of tin silicon oxide precursors. Hydrochloric acid, deionized water, trimethoxy[3-(phenylamino)propyl]silane (PHAPTMS), crystalline tin tetrachloride (SnCl 4 ·5H 2 O) mixed with tetraethyl orthosilicate (TEOS), stirred at room temperature until a homogeneous solution was formed. The final molar composition is 1.0SiO 2 :x SnO 2 (x=0.008, 0.01 and 0.0125): 20H 2 O:0.15HCl:0.08PHAPTMS. The solution was passed through an aerosol spray drying device (BILON-6000Y, drying temperature is 483K) to obtain a white powder. The powder was dried at 383K for 3h to obtain a tin silicon oxide sample.

Embodiment 2

[0052] Synthesis of Sn-Beta molecular sieves. Weigh 1g of the tin-silicon precursor that is not doped with organosilane and add it to a certain amount of template agent tetraethylammonium hydroxide (TEAOH, 40wt%) and hydrofluoric acid solution (HF, 40wt%), and add a certain amount of Beta Seed. After mixing well, put the gel in an oven at 353K for a period of time to remove part of the water. The composition of the final gel is 1.0SiO 2 :0.008SnO 2 :0.4TEA + :0.4F - :2H 2 O: 3 wt% seed crystals. The above gel was transferred to a hydrothermal synthesis kettle with a 10 mL polytetrafluoroethylene liner, and statically crystallized at 443K for 4 days. The crystallized sample was filtered and washed until neutral, dried overnight at 383K, and finally calcined at 813K for 10h in air atmosphere to obtain the product.

Embodiment 3

[0054] Synthesis of Sn-Beta molecular sieves. Weigh 1g of organosilane-doped tin-silicon precursor and add it to a certain amount of template agent tetraethylammonium hydroxide (TEAOH, 40wt%) and hydrofluoric acid solution (HF, 40wt%), and add a certain amount of Beta crystal kind. After mixing well, put the gel in an oven at 353K for a period of time to remove part of the water. The composition of the final gel is 1.0SiO 2 :0.008SnO 2 :0.02PHAPTMS:0.4TEA + :0.4F - :2H 2 O: 3 wt% seed crystals. The above gel was transferred to a hydrothermal synthesis kettle with a 10 mL polytetrafluoroethylene liner, and statically crystallized at 443K for 4 days. The crystallized sample was filtered and washed until neutral, dried overnight at 383K, and finally calcined at 813K for 10h in air atmosphere to obtain the product.

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Abstract

The invention belongs to the technical field of petrochemical engineering, and provides a hydrothermal synthesis method of a nano Sn-Beta molecular sieve aggregate. Hydrophilic organosilane is directly doped into tin-silicon oxide by using an aerosol technology, and is used as a precursor to be mixed with tetraethylammonium hydroxide and hydrofluoric acid for crystallization. The organosilane is trimethoxy[3-(phenylamino)propyl]silane. According to the synthesis method disclosed by the invention, organosilane is pre-dispersed in tin-silicon oxide in advance, so that the problem that organosilane is insoluble in a synthesis system is avoided. Compared with a traditional Sn-Beta molecular sieve, the obtained nano Sn-Beta aggregate in the Baeyer-Villiger oxidation reaction of ketones and hydrogen peroxide has the catalytic performance obviously improved.

Description

technical field [0001] The invention belongs to the technical field of petrochemical industry, and in particular relates to a hydrothermal synthesis method for preparing nano Sn-Beta molecular sieve aggregates. Background technique [0002] Zeolite molecular sieve is a kind of 4 A class of microporous, crystalline aluminosilicate materials composed of tetrahedrons (T represents Si and Al atoms). This material is suitable for heterogeneous catalytic reactions due to its large specific surface area, suitable acidity and channel shape selectivity. has been widely used. In the 1960s, people applied silica-alumina zeolite molecular sieves to catalytic cracking reactions, creating a new era in which molecular sieves catalyze organic heterogeneous reactions. Since then, a large number of researchers have studied the synthesis, characterization and catalytic performance of molecular sieves. In 1983, the Italian scholar Taramasso first synthesized the molecular sieve TS-1 with MFI...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/46C01B39/08
CPCC01B39/46C01B39/08C01P2002/72C01P2002/82C01P2004/03C01P2004/04C01P2002/84
Inventor 熊光孟庆润
Owner DALIAN UNIV OF TECH
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