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Method for the direct synthesis of iron-containing AEI-zeolite catalyst

A zeolite, direct technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve problems such as undiscussed effects of alkali metals, inability to transfer, etc.

Active Publication Date: 2018-12-21
HALDOR TOPSOE AS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the effect of alkali metals was not discussed
Furthermore, this patent application only focuses on the use of copper as a promoter metal ion, so this effect cannot be transferred to catalytic systems with other promoter metal ions

Method used

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  • Method for the direct synthesis of iron-containing AEI-zeolite catalyst
  • Method for the direct synthesis of iron-containing AEI-zeolite catalyst
  • Method for the direct synthesis of iron-containing AEI-zeolite catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0097] Example 1: Synthesis of AEI zeolite (Na-containing material)

[0098] 4.48 g of a 7.4% by weight aqueous solution of N,N-dimethyl-3,5-dimethylpiperidinium hydroxide were mixed with 0.34 g of a 20% by weight aqueous solution of sodium hydroxide (granular NaOH, Scharlab). The mixture was kept under stirring for 10 minutes for homogenization. Thereafter, 0.386g of FAU zeolite (FAU, Zeolyst CBV-720, wherein SiO 2 / Al 2 o 3 =21) was added to the synthesis mixture and kept under stirring for the required time to evaporate excess water until the desired gel concentration was achieved. The final gel composition is SiO 2 :0.047Al 2 o 3 :0.4DMDMP:0.2NaOH:15H 2 O. The resulting gel was filled into a Teflon-lined stainless steel autoclave. Crystallization was then carried out at 135° C. for 7 days under static conditions. The solid product was filtered, washed with copious amounts of water, dried at 100°C and finally calcined in air at 550°C for 4 hours.

[0099] The s...

Embodiment 2

[0100] Example 2: Direct synthesis of Fe-containing AEI structures (materials containing Na)

[0101] 1.98 g of a 7.0% by weight aqueous solution of N,N-dimethyl-3,5-dimethylpiperidinium hydroxide were mixed with 0.24 g of a 20% by weight aqueous solution of sodium hydroxide (granular NaOH, Scharlab). The mixture was kept under stirring for 10 minutes for homogenization. Thereafter, 0.303g of FAU zeolite (FAU, Zeolyst CBV-720, wherein SiO 2 / Al2O 3 =21) was added to the synthesis mixture. Finally, 0.11 g of 20% by weight iron(III) nitrate [Fe(NO 3 ) 3 , Sigma Aldrich, 98%] in water and the synthesis mixture was kept under stirring for the required time to evaporate excess water until the desired gel concentration was achieved. The final gel composition is SiO 2 :0.047Al 2 o 3 :0.01Fe:0.2DMDMP:0.2NaOH:15H 2 O. The resulting gel was filled into a Teflon-lined stainless steel autoclave. Crystallization was then carried out at 140° C. for 7 days under static condition...

Embodiment 3

[0102] Example 3: Synthesis of Fe-containing Na-free AEI zeolites by post-synthesis ion exchange

[0103] First, at 80 °C, the Na-containing AEI material from Example 1 was mixed with 0.1 M ammonium nitrate solution (NH 4 NO 3 , Fluka, 99% by weight) exchange. Then, 0.1 g of ammonium-exchanged AEI zeolite was dispersed in 10 mL of deionized water with 0.1 M HNO 3 Adjust the pH to 3. The suspension was heated to 80 °C under a nitrogen atmosphere, and then 0.0002 mol of FeSO was added 4 .7H 2 O, and the resulting suspension was kept at 80 °C for 1 h with stirring. Finally, the samples were filtered, washed and calcined at 550°C for 4 hours. The final iron content in the sample was 0.9% by weight and the Na content was below 0.04% by weight.

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Abstract

A method for the direct synthesis of a crystalline material with the AEI zeolithic structure containing iron-species and being essentially free of alkali ions, comprising the following steps: (i) preparation of a mixture containing water, a high-silica zeolite as a main source of silica and alumina, an alkyl-substituted cyclic ammonium cation as organic structure directing agent (OSDA), a source of iron, and a source of an alkali metal ion [Alk], to obtain a final synthesis mixture having the following molar composition: SiO2 : a AI2O3 : b Fe : c OSDA : d Alk : e H2O wherein a is in the rangefrom 0.001 to 0.2; wherein b is in the range from 0.001 to 0.2; wherein c is in the range from 0.01 to 2; wherein d is in the range from 0.001 to 2; wherein e is in the range from 1 to 200; (ii) crystallization of the mixture achieved in (i); (iii) recovery of the crystalline material achieved in (ii); (iv) calcination of the crystalline material from step (iii); and (v) removal of the alkali metal cation, present in the calcined crystalline material after step (iv) to obtain a final molar composition: SiO2 : o AI2O3 : p Fe : q Alk wherein o is in the range from 0.001 to 0.2, p is in the rangefrom 0.001 to 0.2 and q is below 0.02.

Description

technical field [0001] The present invention relates to a method for the direct synthesis of crystalline zeolite catalysts having an AEI framework structure comprising iron species. Background technique [0002] Zeolites are microporous crystalline materials composed of horn-shared TO 4 Tetrahedron (T=Si, Al, P, Ti, Ge, Sn, etc.) is formed, and its formation has a molecular size range Micropores and cavities of uniform size and shape. Since the micropores have the same size as small molecules, zeolite materials can be used as molecular sieves. The isomorphic substitution of tetravalent Si in the zeolite framework with elements with different valences (e.g., trivalent) results in the formation of cations (e.g., H + 、Na + 、K + , Ca 2+ etc.) to compensate for the charge imbalance. Charge balancing cations can be exchanged for other cations. This is why zeolites are useful in ion exchange applications. Zeolites can be used as solid Bronsted acids when the charge-bala...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B01J29/76C01B39/06C01B39/48
CPCB01J29/76C01B39/026B01J37/0246B01D53/9418B01J29/7615B01J29/763C01B39/065B01D2251/2062B01D2255/2027B01D2255/20738B01D2255/50B01J2229/183B01J2229/186C01B39/48C01B39/04B01J37/0018C01P2002/60C01P2002/72
Inventor N·马丁加西亚M·莫里尼尔马丁A·考尔玛卡诺斯J·R·托格森P·N·R·温尼斯特罗姆
Owner HALDOR TOPSOE AS