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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

AI Technical Summary

Problems solved by technology

For example, the above method involves an ion exchange step to remove excess copper content and several process steps including crystallization of the final product at about 150°C and high pressure, which results in high energy consumption

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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Effect test

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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