# US 9,517,461 B2 · Ferrous zeolite, method for producing ferrous zeolites, and method for catalytically reducing nitrous oxides

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- Number: US 9,517,461 B2
- Document ID: US9517461B2
- Status: Granted
- Kind: B2
- Application number: 13/516,865
- Filed: 2010-12-13
- Published: 2013-01-03
- Granted: 2016-12-13
- Earliest claimed: 2009-12-18
- Assignees: BASF SE
- Applicants: Dirk A. Grossschmidt; Bilge Yilmaz; Dirk Klingler; Bernd Zoels
- Inventors: Dirk A. Grossschmidt; Bilge Yilmaz; Dirk Klingler; Bernd Zoels
- Web page: https://patentgrep.com/patent/US9517461B2

## CPC

- B01J 37/0238: {via the gaseous phase-sublimation}
- B01D 53/9427: {for removing nitrous oxide}
- B01J 29/072: Iron group metals or copper
- B01J 29/76: Iron group metals or copper
- B01J 29/7615: {Zeolite Beta}
- B01J 29/763: {CHA-type, e.g. Chabazite, LZ-218}
- B01J 29/85: Silicoaluminophosphates [SAPO compounds]
- B01J 37/0234: {Impregnation and coating simultaneously}
- B01D 2251/2062: Ammonia
- B01D 2255/20738: Iron
- B01D 2255/50: Zeolites
- B01J 35/396: {Distribution of the active metal ingredient}
- B01J 35/613: {10-100 m2/g}
- B01J 35/615: {100-500 m2/g}
- B01J 35/643: {less than 2 nm}
- B01J 37/086: {Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid}
- B01J 2229/186: not in framework positions
- B01J 2229/34: Reaction with organic or organometallic compounds
- B01J 2229/40: Special temperature treatment, i.e. other than just for template removal
- Y02C 20/10: of nitrous oxide (N2O)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- Y02C: CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]

## Abstract

Described is an iron-containing zeolite wherein the number of iron sites, based on the zeolite, is greater than the number of cationic positions in the zeolite. Also described is an iron-containing zeolite preparable by gas phase reaction with iron pentacarbonyl, said zeolite having a greater specific surface area than iron-containing zeolites prepared analogously by ion exchange and/or being more hydrothermally stable than iron-containing zeolites prepared analogously by ion exchange, or wherein the number of iron clusters larger than 10 nm is less than 15% by weight, based on the total amount of iron. Further described is a process for preparing an iron-containing zeolitic material, which comprises doping with iron by means of a gas phase reaction using iron pentacarbonyl. Further described is a process for catalytic reduction of nitrogen oxides using catalysts comprising said iron-containing zeolitic materials.

## Claims

### Claim 1

A process for preparing an iron-containing zeolitic material comprising a topology selected from the group consisting of BEA, CHA, and LEV, the method comprising doping a starting zeolitic material with iron by a gas phase reaction comprising:
(i) gas phase loading by flowing iron pentacarbonyl through the starting zeolitic material to provide a zeolitic material laden with iron pentacarbonyl;
(ii) thermal decomposition of the zeolitic material laden with iron pentacarbonyl to provide an iron-containing zeolitic material; and
(iii) flowing steam, air or an inert gas through the iron-containing zeolitic material at temperatures of 500 to 1000° C. at a pressure of 0.1 to 10 bar.

### Claim 2 (depends on 1)

The process according to claim 1, wherein, in component step (i), gaseous iron pentacarbonyl at a concentration of iron pentacarbonyl in the gas stream of 0.1 to 100% by volume is flowed through the starting zeolitic material at a temperature of 10 to 250° C. and a pressure of 0.1 to 10 bar for a period of 0.1 min to 10 h.

### Claim 3 (depends on 1)

The process according to claim 1, wherein, in component step (ii), a gas selected from the group consisting of at least one inert gas, air and combinations thereof is flowed through the zeolitic material laden with iron pentacarbonyl, the temperature in step (ii) being 10 to 500° C., the pressure 0.1 to 10 bar and the reaction time 0.1 min to 10 h.

### Claim 4 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material has a pore diameter less than 0.7 nm.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the iron-containing zeolitic material comprises a topology selected from the group consisting of CHA and LEV.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material has a specific BET surface area of 10 to 1000 g/m2.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material has a specific BET surface area of 150 to 800 g/m2.

### Claim 8 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material has a specific BET surface area of 300 to 700 g/m2.

### Claim 9 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material comprises a silicon dioxide-aluminum oxide ratio greater than 1.

### Claim 10 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material comprises a silicon dioxide-aluminum oxide ratio of 3 to 500.

### Claim 11 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material comprises a silicon dioxide-aluminum oxide ratio of 6 to 60.

### Claim 12 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material has a mean pore diameter of 0.2 to 2 nm.

### Claim 13 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material has a mean pore diameter of 0.3 to 1 nm.

### Claim 14 (depends on 1)

The process according to claim 1, wherein the starting zeolitic material has a mean pore diameter of 0.35 to 0.8 nm.

### Claim 15 (depends on 5)

The process according to claim 5, wherein the iron-containing zeolitic material comprises a CHA topology, and steam is flowed through the iron-containing zeolitic material in step (iii).