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Ionothermal post-synthesis for synthesis of functional heteroatomic molecular sieve

A technology of heteroatom molecular sieve and synthesis method, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, catalyst carriers, etc. It can solve the problems of tin sources that are easy to agglomerate, difficult to disperse, and difficult to control, and achieve low volatility and increase controllable variables , the effect of reducing the risk of stress

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

Taking tin-containing heteroatom molecular sieves as an example, the document J.Phys.Chem.C, dx.doi.org / 10.1021 / jp1076966 prepared Sn-Beta molecular sieves by replacing the Beta molecular sieves dealuminated with nitric acid with SnCl4 gas-phase crystals, but The gas-phase crystal substitution method has the disadvantages of being difficult to operate and difficult to control
Document Angew.Chem.Int.Ed., DOI: 10.1002 / anie.201206193I. Then the Beta molecular sieve through nitric acid dealumination is carried out the research of post-synthesis method by solid-state ion exchange, but this method exists that the tin source used is easy The obvious disadvantages of agglomeration and not easy to disperse

Method used

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  • Ionothermal post-synthesis for synthesis of functional heteroatomic molecular sieve
  • Ionothermal post-synthesis for synthesis of functional heteroatomic molecular sieve
  • Ionothermal post-synthesis for synthesis of functional heteroatomic molecular sieve

Examples

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Effect test

Embodiment 1

[0047]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).

[0048] 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 :.

[0049] 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

[0051] 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).

[0052] 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 .

[0053] 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

[0055] 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).

[0056] Then in a reactor, take by weighing 100g of dissolved 1-butyl-3-methyl imidazolium chloride salt ionic liquid, add 0.07g of titanium tetrachloride and stir it vigorously 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 :0.01TiO 2 .

[0057] 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 Ti-MWW molecular sieve. The reaction product has carried out the ...

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Abstract

An ionthermal post-synthesis method for synthesis of a functional heteroatomic molecular sieve is as follows: a heteroatomic precursor compound, ionic liquid and a parent molecular sieve are mixed evenly according to a certain proportion and feeding method for crystallization for a certain time at a certain temperature, the corresponding functional heteroatomic molecular sieve can be obtained by separating, washing and drying, and the heteroatom content range of the synthesized functional heteroatomic molecular sieve is within 0.001 to 0.1. The crystallization product can be used directly as a catalyst or a catalyst carrier. The method has universality, on the one hand, the method can be used for synthesis of the l heteroatomic molecular sieve difficult to obtain by hydrothermal synthesis, on the other hand, the ionic liquid can be recycled, and the method has the advantages of simple operation, and easy industrial application.

Description

technical field [0001] The invention relates to an ion thermal post-synthesis method of molecular sieves. In particular, the present invention relates to a method for the preparation of functional heteroatom 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. Later researchers discovered a series of germanate-based molecular sieves. Molecular sieve materials have special shape-selective catalytic properties due to their uniform composition, regular structure, adjustable surface acidity and molecular pore size, and are used as catalytic materials, gas separation and adsorbents, ion exchangers, etc. in petroleum It has been widely used in the fields of natural gas processing, fine chemicals, environmental protection and nuclear waste treatment. [0003] Since different chemical reactions have differe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/70B01J29/86B01J29/89B01J29/18B01J29/84B01J32/00
Inventor 王炳春田志坚马怀军曲炜徐竹生李鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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