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

A topological structure and molecular sieve technology, which is applied in molecular sieve catalysts, chemical instruments and methods, catalyst carriers, etc., can solve the problems of easy agglomeration, difficult control, and difficult dispersion of tin sources, and achieve low volatility, increase controllable variables, and good The effect of catalytic performance

Active Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For tin-containing heteroatom molecular sieves, P.Wu et al. used gas-phase SnCl 4 Study on Synthetic Method after Isomorphic Substitution / jp1076966], but the gas-phase crystal substitution method has the disadvantages of being difficult to operate and difficult to control
I.Hermans etc. carry out the research [C.Hammond, S.Conrad, and I.Hermans, Angew.Chem.Int.Ed., DOI: 10.1002 / anie.201206193], this method has obvious disadvantages that the tin source used is easy to agglomerate and difficult to disperse

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Treat 3 g of Beta molecular sieve (silicon-aluminum ratio = 21) 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 Beta molecular sieve (silicon Aluminum ratio>2000).

[0037] 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- Beta 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 :0.1SnO 2 .

[0038] 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 is completed, the reactant is cooled to room temperature, filtered, washed and dried to obtain a tin-containing Beta heteroatom molecular sieve. The react...

Embodiment 2

[0040] Treat 3 g of borosilicate Beta molecular sieve (silicon-boron ratio = 25) with concentrated nitric acid (concentration 65%) at a liquid:solid ratio (weight ratio) of 20 for 10 hours under ultrasonically strengthened heating at 100°C to obtain Si-rich Beta molecular sieve of -OH (silicon to boron ratio>1300).

[0041] 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 Beta molecular sieve rich in Si-OH 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 .

[0042] 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 is completed, the reactant is cooled to room temperature, filtered, washed and ...

Embodiment 3

[0044] 3 g of pure silicon Beta molecular sieves were treated with tetraethylammonium hydroxide (concentration 25%) at a liquid:solid ratio of 20 (weight ratio) under microwave-enhanced heating at 50°C for 10 hours to obtain Si-OH-rich Beta molecular sieve.

[0045] Then in a reactor, take by weighing 100g of dissolved 1-butyl-3-ethylbromoimidazolium salt ionic liquid, add tin tetrachloride 0.02g and vigorously stir for 4 hours, then add the Si-rich Si- Beta 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 :0.001SnO 2 .

[0046] The prepared crystallization mixture was evenly mixed and then transferred to an open reaction kettle for crystallization under microwave-enhanced heating at 180° C. for 2 hours. After the crystallization is completed, the reactant is cooled to room temperature, filtered, washed and dried to obtain a tin-containing Beta heteroatom molecula...

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Abstract

The present invention discloses a tin-containing heteroatomic functional molecular sieve with a BEA topologic structure and a synthesis method thereof, the tin-containing heteroatomic functional molecular sieve has the characteristics of the BEA topologic structure, silicon-tin ratio (atomic ratio) of the Sn-beta heteroatomic functional molecular sieve is in the range of 10 to 1000, and the synthesis method of the tin-containing beta molecular sieve is an ionothermal secondary synthesis preparation method. A tin source, ionic liquid and a beta 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-beta 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-beta 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 BEA topological structure characteristics and a preparation method thereof. In particular, the present invention relates to a method for preparing tin-containing Beta molecular sieves by ion thermal 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 i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/70B01J32/00
Inventor 王炳春田志坚马怀军曲炜李鹏徐竹生
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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