One-pot synthesis of copper-containing small-pore zeolites

A technology of zeolite and faujasite zeolite is applied in the field of preparing copper-containing small-pore zeolite, and can solve problems such as high energy consumption

Active Publication Date: 2021-07-30
UMICORE AG & CO KG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the above method involves an ion exchange step to remove excess copper content and several process step...

Method used

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  • One-pot synthesis of copper-containing small-pore zeolites
  • One-pot synthesis of copper-containing small-pore zeolites

Examples

Experimental program
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Embodiment 1

[0048] a) Synthesis of Cu-tetraethylenepentylamine complex (Cu-TEPA): 37.9g ​​tetraethylenepentylamine (0.2 mole) was added to 50g CuSO 4 ·5H 2 O (0.2 mol) in 200g H 2 O in solution (1M solution), then kept stirring at room temperature for 2 hours.

[0049] b) 3 g of SAR=30 (Si / Al=15) zeolite Y (CBV720 supplied by Zeolyst International) were suspended in 27 mL of 1.2 M sodium hydroxide solution. To this solution was added 1.5 mL of 1M Cu-TEPA solution. The final colloid has the following molar ratios: 1 SiO 2 / 0.033 Al 2 o 3 / 0.033 Cu-TEPA / 0.70 NaOH / 34H 2 O. The suspension was stirred at room temperature for 10 minutes before being transferred to an oven at 95 °C and left to stand for 7 days. After cooling to room temperature, the powder was isolated from the mother liquor by filtration, washed with deionized water and dried at 60 °C for 12 h. Generated zeolite according to the X-ray diffraction pattern (see figure 1 ) was determined to have a CHA framework type code...

Embodiment 2

[0052] 1.5 g of zeolite Y of SAR=30 (Si / Al=15) (CBV720 supplied by Zeolyst International) and 1.5 g of zeolite Y of SAR=5.1 (Si / Al=2.55) (CBV300 supplied by Zeolyst International) The mixture was suspended in 27 mL of 1.2 M potassium hydroxide solution. To this solution was added 3 mL of 1M Cu-TEPA solution. The final colloid has the following molar ratios: 1 SiO 2 / 0.10Al 2 o 3 / 0.076 Cu-TEPA / 0.82 KOH / 42H 2 O. The suspension was stirred at room temperature for 10 minutes before being transferred to an oven at 95 °C and left to stand for 5 days. After cooling to room temperature, the powder was isolated from the mother liquor by filtration, washed with deionized water and dried at 60 °C for 12 h. The resulting zeolite was determined to have a CHA framework type code with a Si / Al ratio of 3.3 and a CuO content of 6.4% by weight.

Embodiment 3

[0054] Example 2 was repeated except that instead of potassium hydroxide, 27 mL of 1.2M sodium hydroxide solution was disclosed. The final colloid has the following molar ratios: 1 SiO 2 / 0.10 Al 2 o 3 / 0.076 Cu-TEPA / 0.82 NaOH / 42H 2 O. The resulting zeolite after 11 days was determined to have a CHA framework type code with a Si / Al ratio of 2.9 and a CuO content of 8 wt%.

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Abstract

The present invention relates to a process for the preparation of copper-containing small pore zeolites, said process comprising: preparing a zeolite comprising a faujasite framework type, Cu-tetraethylenepentylamine (Cu-TEPA) and at least one compound M(OH )x, the mixture not comprising tetraethylammonium cations, and heating the reaction mixture to form a copper-containing small pore zeolite.

Description

technical field [0001] The present invention relates to a process for the preparation of copper-containing small pore zeolites in a one-step synthesis. Background technique [0002] Zeolites are microporous aluminosilicate materials that have a very regular molecular-sized pore structure and occur in a variety of framework structures. The Structure Commission of the International Zeolite Association classifies zeolites and defines the corresponding framework types. The committee also assigns a three capital letter skeleton type code to all unique and confirmed skeleton topologies. For example, a group of widely used zeolites belongs to the faujasite framework which has been assigned the code FAU. [0003] Zeolites are also often classified according to their pore size, which is defined by the ring size of the largest pore opening. Large pore zeolites have a maximum ring size of 12 tetrahedral atoms, medium pore zeolites have a maximum pore size of 10 tetrahedral atoms, an...

Claims

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Application Information

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IPC IPC(8): B01J29/76C01B39/48
CPCB01J29/76B01J29/763C01B39/02C01B39/026C01B39/06B01D53/9418B01D2255/50B01D2257/404B01D2258/01B01J29/072B01J29/08B01J29/56B01J29/7607B01J2229/18B01J2229/183B01J2229/186B01J2229/20B01J2229/34B01J2229/40
Inventor J·A·马滕斯S·P·斯里S·J·P·克尔克霍夫斯E·J·J·费尔海恩F-W·许策
Owner UMICORE AG & CO KG
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