# US 10,500,573 B2 · Zeolite synthesis with alkaline earth metal

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- Number: US 10,500,573 B2
- Document ID: US10500573B2
- Status: Granted
- Kind: B2
- Application number: 15/718,624
- Filed: 2017-09-28
- Published: 2018-04-05
- Granted: 2019-12-10
- Earliest claimed: 2016-09-30
- Assignees: Johnson Matthey Public Limited Company
- Applicants: Johnson Matthey Public Limited Company
- Inventors: Hai-Ying Chen; Joseph Fedeyko; Raul Lobo; Nicholas McNamara; Trong Pham
- Web page: https://patentgrep.com/patent/US10500573B2

## CPC

- B01J 29/78: containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01D 53/94: by catalytic processes
- B01D 53/9413: {Processes characterised by a specific catalyst}
- B01D 53/9418: {for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas}
- B01D 53/9422: {for removing nitrogen oxides by NOx storage or reduction by cyclic switching between lean and rich exhaust gases (LNT, NSC, NSR)}
- B01D 53/944: {Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts (three-way-catalysts [TWC] B01D53/9445)}
- B01J 20/18: Synthetic zeolitic molecular sieves
- B01J 29/70: of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J 29/72: containing iron group metals, noble metals or copper
- B01J 29/74: Noble metals
- B01J 29/76: Iron group metals or copper
- B01J 35/19: {Catalysts containing parts with different compositions}
- B01J 35/56: Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional [3D] monoliths
- B01J 35/77: Compounds characterised by their crystallite size
- B01J 37/0018: {Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)}
- B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/10: in the presence of water, e.g. steam
- B01J 37/30: Ion-exchange
- C01B 39/026: {After-treatment}
- C01B 39/04: using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
- C01B 39/08: the aluminium atoms being wholly replaced
- C01B 39/48: using at least one organic template directing agent
- B01D 2255/1023: Palladium
- B01D 2255/2042: Barium
- B01D 2255/2045: Calcium
- B01D 2255/2047: Magnesium
- B01D 2255/2092: Aluminium
- B01D 2255/30: Silica
- B01D 2255/50: Zeolites
- B01D 2255/91: NOx-storage component incorporated in the catalyst
- B01D 2255/915: Catalyst supported on particulate filters
- B01D 2255/9155: Wall flow filters
- B01D 2258/012: Diesel engines and lean burn gasoline engines
- B01J 2229/183: in framework positions
- B01J 2229/186: not in framework positions
- B01J 2235/00: Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
- B01J 2235/15: X-ray diffraction
- B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/03: obtained by SEM
- F01N 3/0222: {the structure being monolithic, e.g. honeycombs}
- F01N 3/035: with catalytic reactors
- F01N 3/0814: {combined with catalytic converters, e.g. NOx absorption/storage reduction catalysts}
- F01N 3/0842: {Nitrogen oxides}
- F01N 3/103: {Oxidation catalysts for HC and CO only}
- F01N 3/2066: {Selective catalytic reduction [SCR]}
- F01N 2330/02: Metallic plates or honeycombs, e.g. superposed or rolled-up corrugated or otherwise deformed sheet metal
- F01N 2370/04: Zeolitic material
- 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)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- F01N: GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL-COMBUSTION ENGINES (arrangements in connection with gas exhaust of propulsion units in vehicles B60K13/00; combustion-air intake silencers specially adapted for, or arranged on, internal-combustion engines F02M35/00; protecting against, or damping, noise in general G10K11/16)

## Abstract

Provided is a novel synthesis technique for producing pure phase small pore zeolites employing a synthesis gel of at least one zeolite, a structure directing agent and an alkaline earth metal source. Additionally provided are a novel form of AFX zeolite, a novel synthesis method for producing a zeolite with an increased Al pair content, a catalyst comprising the AFX zeolite in combination with a metal, and methods of using the same.

## Claims

### Claim 1

A method for making an aluminosilicate zeolite having a small pore framework comprising reacting a synthesis gel comprising at least one zeolite, a structure directing agent, an alkaline earth metal source, and an optional silica source at a temperature of at least about 100° C. until crystals of the small pore zeolite form.

### Claim 2 (depends on 1)

The method of claim 1, wherein the small pore zeolite crystals are at least about 90% phase pure.

### Claim 3 (depends on 1)

The method of claim 1, wherein the synthesis gel is substantially free of alkaline metal.

### Claim 4 (depends on 1)

The method of claim 1, wherein the synthesis gel has one or more of the following compositional molar ratios:
SiO2/Al2O3 of about 10 to about 80;
Na2O/Al2O3 of about 0 to about 2;
MAEO/Al2O3 of about 0.3 to about 1.5 (MAE can be Ca, Sr, or Ba);
SDA2O/Al2O3 of about 0.7 to about 20;
H2O/Al2O3 of about 300 to about 3000; and
OH−/SiO2 of about 0.25 to about 0.5.

### Claim 5 (depends on 1)

The method of claim 1, wherein the SDA cation is 1,3-bis(1-adamantyl)imidazolium, N,N-diethyl-cis 2,6-dimethylpiperidinium, N,N-dimethyl-3,5-dimethylpiperidinium, N,N,N-1-trimethyladamantylammonium, or N,N,N-dimethylethylcyclohexylammonium.