One-pot method for the synthesis of cu-ssz-13, the compound obtained by the method and use thereof

A technology of cu-ssz-13 and mixture, applied in molecular sieves and base exchange compounds, separation methods, chemical instruments and methods, etc., can solve problems such as uncontrollable Si/Al ratio and Cu content

Active Publication Date: 2015-07-29
UMICORE AG & CO KG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the direct synthesis based on Cu-TEPA complex as a unique OSDA for the preparation of SSZ-13 cannot control the Si / Al ratio and Cu content

Method used

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  • One-pot method for the synthesis of cu-ssz-13, the compound obtained by the method and use thereof
  • One-pot method for the synthesis of cu-ssz-13, the compound obtained by the method and use thereof
  • One-pot method for the synthesis of cu-ssz-13, the compound obtained by the method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Embodiment 1: Synthesis of N, N, N-trimethyl-1-adamantyl ammonium

[0056] 29.6 grams of 1-adamantanamine (Sigma-Aldrich) and 64 grams of potassium carbonate (Sigma-Aldrich) were mixed with 320 ml of chloroform. At this point, 75 g of iodomethane was added dropwise while the reaction was stirring in an ice bath. The reaction was kept under stirring at room temperature during the 5 days. The mixture was filtered and washed with diethyl ether, and the resulting solid was further extracted with chloroform. The final product is N,N,N-trimethyl-1-adamantyl ammonium iodide. The iodide salt is anion exchanged with an ion exchange resin to obtain the hydroxide form.

Embodiment 2

[0057] Example 2: Direct synthesis of "Cu-SSZ13-1" in OH medium

[0058] 159 mg of a 20 wt% aqueous solution of copper(II) sulfate (98 wt%, Alfa) was mixed with 36 mg of tetraethylenepentamine (TEPA, 99 wt%, Aldrich) and kept stirring for 2 hours. Subsequently, 1041 mg of an aqueous solution of N,N,N-trimethyl-1-adamantyl ammonium hydroxide (TMaDA, 16% by weight) and 95 mg of an aqueous solution of sodium hydroxide (20% by weight) were added and kept stirring for 15 minute. 21 mg of aluminum hydroxide (66% by weight, Sigma-Aldrich) and 607 mg of colloidal silicon dioxide (Ludox AS40, 40% by weight, Aldrich) were then introduced into the synthesis mixture and kept stirring for the required time to evaporate the Solvent until desired gel concentration. The final gel composition is SiO 2 :0.033Al 2 o 3 :0.049Cu(TEPA) 2+ :0.19TMaDA:0.12NaOH:18.3H 2 O.

[0059] The gel was transferred to a Teflon-lined autoclave and heated to a temperature of 150° C. under static conditions...

Embodiment 3

[0062] Example 3: Direct synthesis of "Cu-SSZ13-2" in OH medium

[0063] 325 mg of a 20 wt% aqueous solution of copper(II) sulfate (98 wt%, Alfa) were mixed with 74 mg of tetraethylenepentamine (TEPA, 99 wt%, Aldrich) and kept stirring for 2 hours. Subsequently, 535 mg of aqueous N,N,N-trimethyl-1-adamantane ammonium hydroxide (TMaDA, 16% by weight) and 161 mg of aqueous sodium hydroxide (20% by weight) were added and stirring was maintained for 15 minutes. 21 mg of aluminum hydroxide (66% by weight, Sigma-Aldrich) and 614 mg of colloidal silicon dioxide (Ludox AS40, 40% by weight, Aldrich) were then introduced into the synthesis mixture and kept stirring for the required time to evaporate the solvent to the desired gel concentration. The final gel composition is SiO 2 :0.033Al 2 o 3 :0.10Cu(TEPA) 2+ :0.10TMaDA:0.20NaOH:19.1H 2 O.

[0064] The gel was transferred to a Teflon-lined autoclave and heated to a temperature of 150° C. under static conditions during 14 days. ...

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Abstract

Process for the direct synthesis of Cu-SSZ-13 from a synthesis mixture comprising water, at least one silicon source, at least one Al source, at least one Cu source, at least one polyamine for complexing with Cu, and a single organic structure directing agent. A Cu containing molecular sieve having the framework structure of SSZ-13, obtainable by the process and use of the Cu containing molecular sieve.

Description

technical field [0001] The present invention relates to a process for the direct preparation of SSZ-13 zeolites containing copper atoms. This new approach requires a specific combination of copper polyamine complexes with additional organic molecules that act as organic structure-directing agents (OSDAs). The present invention also includes using the Cu-SSZ-13 material synthesized according to the method of the present invention as NO x A method of selective catalytic reduction (SCR) catalysts. Background technique [0002] Zeolites are composed of TO interconnected by oxygen atoms 4 Microporous materials composed of tetrahedrons (T=Si, Al, P, Ti, Ge, Sn...), which generate pores and cavities of uniform size and shape (in the molecular scale range Inside). [0003] Barrer described the first synthetic zeolites in 1948. [Barrer, J. Chem. Soc. 127 (1948)]. Since this discovery, more than 200 new zeolite structures have been discovered, all of which contain different por...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/94B01J29/06C01B39/48
CPCC01B39/48B01D53/9418B01D2255/50C01B39/06B01J29/763B01D2255/20761B01D53/04B01J29/064B01D53/8628B01J29/76B01J37/0018B01J37/10
Inventor M·M·马林R·M·弗兰科A·C·卡诺斯J·R·托格森
Owner UMICORE AG & CO KG
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