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Method for preparing the silicoaluminate form of the aei zeolite structure with high yields, and application in catalysis of method

A technology of zeolite and zeolite materials, applied to the high-yield preparation of aluminosilicates with AEI zeolite structure, can solve the problem of completely eliminating complexities

Inactive Publication Date: 2018-01-26
CONSEJO SUPERIOR DE INVESTIGACIONES CIENTIFICAS (CSIC) +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, this method requires the use of phosphine-derived OSDA, which exhibits significant disadvantages
On the one hand, the use of organic molecules derived from phosphines raises serious, unavoidable environmental and health concerns
On the other hand, the complete elimination of phosphorus species remaining in the zeolite cavity is very complicated, especially in small pore zeolites, and the elimination process requires a calcination step at very high temperature and hydrogen atmosphere to completely decompose / eliminate all phosphorus species. The above substances (Sonoda, et al. J. Mater. Chem. A, 2015, 3, 857)

Method used

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  • Method for preparing the silicoaluminate form of the aei zeolite structure with high yields, and application in catalysis of method
  • Method for preparing the silicoaluminate form of the aei zeolite structure with high yields, and application in catalysis of method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Example 1: Synthesis of N,N-dimethyl-3,5-dimethylpiperidinium (DMDMP)

[0070] Mix 10 g of 3,5-dimethylpiperidine (Sigma-Aldrich, ≥96% by weight) with 19.51 g of potassium bicarbonate (KHCO 3 , Sigma-Aldrich; 99.7% by weight) were mixed and dissolved in 140 ml of methanol. Subsequently, 54ml methyl iodide (CH 3 I, Sigma-Aldrich, > 99% by weight), the resulting mixture was kept stirring at room temperature for 5 days. Once this time had elapsed, the reaction mixture was filtered to remove potassium bicarbonate. The filtered solution was partially concentrated by rotary evaporator. Once the methanol was partially evaporated, the solution was washed several times with chloroform and magnesium sulfate (MgSO 4 , Sigma-Aldrich, > 99.5% by weight). Subsequently, the mixture was filtered to remove magnesium sulfate. The ammonium salt was obtained by precipitation with diethyl ether followed by filtration. The final yield of N,N-dimethyl-3,5-dimethylpiperidinium iodide wa...

Embodiment 2

[0072] Example 2: Synthesis of an aluminosilicate form of the AEI zeolite structure using a zeolite with the FAU structure as the sole source of silicon and aluminum

[0073] 21.62 g of a 6.9% by weight aqueous solution of N,N-dimethyl-3,5-dimethylpiperidinium hydroxide were mixed with 1.89 g of a 20% by weight aqueous sodium hydroxide solution (NaOH, Sigma-Aldrich, 98%) mixed. The mixture was homogenized by maintaining stirring for 10 minutes. Finally, 3.01 g of zeolite (CBV-720, SiO 2 / Al 2 o 3 molar ratio = 21), and the mixture was kept stirring until the desired concentration was reached. The composition of the final gel is SiO 2 / 0.047Al 2 o 3 / 0.2DMDMP / 0.2NaOH / 15H 2 O. The gel was transferred to a Teflon-lined steel autoclave and heated at 135 °C under static conditions for 7 days. Once this time has elapsed, the resulting product is recovered by filtration, washed well with water and finally dried at 100°C. The material was calcined at 550° C. for 4 hours in ...

Embodiment 3

[0075] Example 3: Synthesis of an aluminosilicate form of the AEI zeolite structure using a zeolite with the FAU structure as the sole source of silicon and aluminum

[0076] 2.24 g of 7.4% by weight of N,N-dimethyl-3,5-dimethylpiperidine hydroxide in water and 0.173 g of 20% by weight of sodium hydroxide in water (NaOH, Sigma-Aldrich, 98 %)mix. The mixture was homogenized by maintaining stirring for 10 minutes. Finally, 0.193 g of zeolite (CBV-720, SiO 2 / Al 2 o 3 molar ratio = 21), and the mixture was kept stirring until the desired concentration was reached. The composition of the final gel is SiO 2 / 0.047Al 2 o 3 / 0.4DMDMP / 0.2NaOH / 15H 2 O. The gel was transferred to a Teflon-lined steel autoclave and heated at 135 °C under static conditions for 7 days. Once this period of time has elapsed, the resulting product is recovered by filtration, washed well with water and finally dried at 100°C. The material was calcined at 550° C. for 4 hours in an air atmosphere to e...

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Abstract

The invention discloses a method for preparing the silicoaluminate form of the AEI zeolite structure with high yields, and application in catalysis of the method. The present invention relates to a new process for synthesising the silicoaluminate form of the AEI zeolite structure based on the use of another zeolite, zeolite Y, as the only source of silicon and aluminum, in order to obtain high synthesis yields (greater than 80%) in the absence of any other source of silicon, phosphine-derivedcationsand fluoride anions in the synthesis medium. The N, N-dimethyl-3,5-dimethylpiperidinium cation may be used as the OSDA, and the FAU crystal structure is transformed into the AEI crystal structure with high yields. It also discloses the preparation of catalysts based on the silicoaluminateform ofthe AEI crystal structure, wherein Cu atoms have been introduced, and the subsequent application thereof as a catalyst, preferably in the SCR of NOx.

Description

[0001] manual technical field [0002] The present invention discloses a new method for the synthesis of the aluminosilicate form of the AEI zeolite structure, based on the use of another zeolite, for example zeolite Y (FAU zeolite structure), as the sole source of silicon and aluminum, to be used in High synthesis yields (higher than 80%) were obtained in the absence of any other sources of silicon, phosphine-derived cations and fluoride anions in the synthesis medium. The present invention also discloses the preparation of the aluminosilicate form of zeolite AEI, synthesized by a post-synthetic method, with Cu species introduced therein, and its use as a catalyst in the Selective Catalytic Reduction (SCR) of NOx, etc. Applications. Background technique [0003] Zeolites or molecular sieves are described as being composed of TO interconnected by oxygen atoms 4 Tetrahedral (T = Si, Al, P, Ge, B, Ti, Sn, etc.) formed material, which has pores and cavities that are uniform i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/48B01J29/76B01J29/70B01D53/86B01D53/56
CPCB01J29/70C01B39/026B01J29/76B01J37/0063B01J2229/186B01J2229/36B01D53/9418B01D2255/50C01B39/48C01B39/023C01B39/04C01B39/24Y02P30/20Y02P30/40B01J35/30B01D53/00B01J29/80C07C1/20C07C11/04C07C2529/072B01D9/0036B01J2229/183
Inventor A·科玛卡诺斯M·莫林内尔马林N·马丁加西亚
Owner CONSEJO SUPERIOR DE INVESTIGACIONES CIENTIFICAS (CSIC)
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