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Tin-containing molecular sieve with MWW topological structure and preparation and application thereof

A topology, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of low tin content, long synthesis time, low crystallinity, etc., and achieve low volatility and good quality. Catalytic performance, the effect of increasing the controllable variable

Active Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

But the paradox is that on the other hand, the radius of tin is much larger than that of silicon, so it is difficult to enter the framework of molecular sieves. Like the synthesis of titanium-silicon molecular sieves, the tin source and alkali metal ions in the sol system will inhibit the formation of tin. Therefore, in fact, the tin-containing MWW molecular sieve obtained by this hydrothermal synthesis system not only has a very low crystallinity, but also has a very low tin content in the system, and the synthesis time is also very long

Method used

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  • Tin-containing molecular sieve with MWW topological structure and preparation and application thereof
  • Tin-containing molecular sieve with MWW topological structure and preparation and application thereof
  • Tin-containing molecular sieve with MWW topological structure and preparation and application thereof

Examples

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Effect test

Embodiment 1

[0034] Treat 3 g of MCM-22 molecular sieve (silicon-aluminum ratio = 25) with concentrated nitric acid (concentration 65%) at 100°C for 24 hours at a liquid:solid ratio (weight ratio) of 20 to obtain Si-OH-rich MWW molecular sieves (Si-aluminum ratio>1900).

[0035] Then in a reactor, take by weighing 100g of dissolved 1-butyl-3-methyl imidazolium chloride ionic liquid, add 1.5g of tin tetrachloride and vigorously stir the reaction for 4 hours, then add the Si-rich Si- The MWW molecular sieve of OH was added, and the reaction was vigorously stirred for 4 hours to obtain a uniformly mixed crystallized mixture with a molar ratio of 1.0 SiO 2 :0.1SnO 2 .

[0036] The prepared crystallization mixture was evenly mixed, then transferred to an open reaction kettle, and crystallized at 200° C. for 20 hours. After the crystallization, the reactant was cooled to room temperature, filtered, washed and dried to obtain a tin-containing MWW heteroatom molecular sieve. The reaction produ...

Embodiment 2

[0038] Treat 3 g of borosilicate MCM-49 molecular sieve (silicon-boron ratio = 25) with concentrated nitric acid (concentration 65%) at a liquid: solid ratio (weight ratio) of 20 under ultrasonically enhanced heating at 100°C for 10 hours to obtain rich MWW molecular sieves containing Si-OH (silicon-boron ratio>800).

[0039] Then in a reactor, weigh 100g of the dissolved 1-ethyl-3-methylimidazolium chloride and tetraethylammonium chloride mixture (weight ratio 1:1) ionic liquid, add 0.15g of tin tetrachloride Stir vigorously for 4 hours, then add the Si-OH-rich MWW molecular sieve obtained above, and stir vigorously for 4 hours to obtain a uniformly mixed crystallized mixture with a molar ratio of 1.0 SiO 2 :0.01SnO 2 .

[0040] The prepared crystallization mixture was evenly mixed and then transferred to a closed reactor for crystallization at 100° C. for 240 hours. After the crystallization, the reactant was cooled to room temperature, filtered, washed and dried to obtai...

Embodiment 3

[0042] Treat 3 g of MCM-56 molecular sieve (silicon-aluminum ratio = 25) under hydrothermal conditions at 550°C for 4 hours, and then use concentrated nitric acid (concentration 65%) at 80°C according to the liquid: solid ratio of 20 (weight ratio) Under treatment for 4 hours, a MWW molecular sieve rich in Si-OH (silicon-aluminum ratio>920) was obtained.

[0043] Then in a reactor, weigh 100 g of dissolved 1-heptyl-3-methylchloropiperidinium salt ionic liquid, add 0.33 g of tin tetrachloride and vigorously stir for 4 hours, and then add the previously obtained Si-rich The MWW molecular sieve of -OH was added, and the reaction was vigorously stirred for 4 hours to obtain a well-mixed crystallized mixture with a molar ratio of 1.0 SiO 2 :0.025SnO 2 .

[0044] The prepared crystallization mixture was evenly mixed, then transferred to an open reaction kettle, and crystallized at 150° C. for 10 hours. After the crystallization, the reactant was cooled to room temperature, filter...

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Abstract

The present invention discloses a tin-containing heteroatomic functional molecular sieve with a MWW topologic structure and a synthesis method thereof, the silicon-tin ratio (atomic ratio) of the Sn-MWW heteroatomic functional molecular sieve is in the range of 10 to 1000, and the synthesis method of the tin-containing MWW molecular sieve is an ionothermal secondary synthesis preparation method. A tin source, ionic liquid and a MWW molecular sieve rich in Si-OH groups are evenly mixed according to a certain proportion and feeding method for crystallization for a certain time at a certain temperature, the Sn-MWW heteroatomic functional molecular sieve can be obtained by separation, washing and drying, and a crystallization product can be directly used as a catalyst or catalyst carrier. The Sn-MWW heteroatomic functional molecular sieve has good catalytic performance in the catalytic conversion of biomass and a plurality of fine chemical reaction processes.

Description

technical field [0001] The invention relates to a tin-containing heteroatom functional molecular sieve with MWW topological structure characteristics and a preparation method thereof. In particular, the present invention relates to a method for preparing tin-containing MWW molecular sieves by ionothermal secondary synthesis. Background technique [0002] Molecular sieves are classified according to their basic composition, mainly silicate-based molecular sieves and phosphate-based molecular sieves. Since different chemical reactions have different requirements on the pore structure and surface properties of porous catalytic materials, on the one hand, the synthesis of new structural molecular sieve materials is always an important research content in materials science and catalytic science; on the other hand, the function of molecular sieve materials The chemical design, synthesis and modification also expand the definition and scope of molecular sieves. Among them, the in...

Claims

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Application Information

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IPC IPC(8): C01B39/08B01J29/89B01J32/00
Inventor 王炳春田志坚马怀军曲炜李大伟徐竹生
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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