# US 10,870,583 B2 · Process for the production of a zeolitic material via solvent-free interzeolitic conversion

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- Number: US 10,870,583 B2
- Document ID: US10870583B2
- Status: Granted
- Kind: B2
- Application number: 16/463,263
- Filed: 2017-12-13
- Published: 2019-10-03
- Granted: 2020-12-22
- Earliest claimed: 2016-12-21
- Assignees: BASF SE
- Applicants: BASF SE
- Inventors: Robert McGuire; Mathias Feyen; Ulrich Mueller; Xinhe Bao; Weiping Zhang; Dirk De Vos; Hermann Gies; Feng-Shou Xiao; Toshiyuki Yokoi; Ute Kolb; Bernd Marler; Chuan Shi; Xiulian Pan; Xiangju Meng; Stefan Maurer; Yu Dai; Yong Wang; Trees De Baerdemaeker
- Web page: https://patentgrep.com/patent/US10870583B2

## CPC

- C01B 39/48: using at least one organic template directing agent
- B01D 53/9418: {for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas}
- B01J 29/06: Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J 29/70: of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J 29/7015: {CHA-type, e.g. Chabazite, LZ-218}
- B01J 29/763: {CHA-type, e.g. Chabazite, LZ-218}
- B01J 35/617: {500-1000 m2/g}
- B01J 35/633: {less than 0.5 ml/g}
- B01J 35/643: {less than 2 nm}
- B01J 35/647: {2-50 nm}
- B01J 35/651: {50-500 nm}
- B01J 35/70: characterised by their crystalline properties, e.g. semi-crystalline (catalysts comprising carbon B01J21/18; molecular sieves B01J29/00)
- B01J 37/08: Heat treatment {(B01J37/0009, B01J37/0018 take precedence)}
- B01J 37/30: Ion-exchange
- C01B 39/026: {After-treatment}
- B01D 53/9427: {for removing nitrous oxide}
- B01D 53/9436: {Ammonia}
- B01D 2253/1085: characterized by a silicon-aluminium ratio
- B01D 2253/306: Surface area, e.g. BET-specific surface
- B01D 2253/311: Porosity, e.g. pore volume
- B01D 2255/50: Zeolites
- B01D 2255/9205: Porosity
- B01D 2255/9207: Specific surface
- B01D 2257/402: Dinitrogen oxide
- B01D 2257/404: Nitrogen oxides other than dinitrogen oxide
- B01D 2257/406: Ammonia
- B01D 2257/504: Carbon dioxide
- B01D 2258/012: Diesel engines and lean burn gasoline engines
- B01J 2229/186: not in framework positions
- B01J 2235/05: Nuclear magnetic resonance [NMR]
- B01J 2235/15: X-ray diffraction
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/86: by NMR- or ESR-data
- Y02C 20/10: of nitrous oxide (N2O)
- Y02P 20/151: Reduction of greenhouse gas [GHG] emissions, e.g. CO2
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02C: CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A process for preparing a zeolitic material containing YO2 and X2O3, where Y and X represent a tetravalent element and a trivalent element, respectively, is described. The process includes (1) a step of preparing a mixture containing one or more structure directing agents, seed crystals, and a first zeolitic material containing YO2 and X2O3 and having FAU-, GIS-, MOR-, and/or LTA-type framework structures; and (2) a step of heating the mixture for obtaining a second zeolitic material containing YO2 and X2O3 and having a different framework structure than the first zeolitic material. The mixture prepared in (1) and heated in (2) contains 1000 wt % or less of H2O based on 100 wt % of YO2 in the framework structure of the first zeolitic material. A zeolitic material obtainable and/or obtained by the process and its use are also described.

## Claims

### Claim 1

A process for preparing a zeolitic material comprising YO2 and X2O3 in its frame-work structure, wherein Y stands for a tetravalent element and X stands for a trivalent element, said process comprising:
(1) preparing a mixture comprising one or more structure directing agents, seed crystals, and a first zeolitic material comprising YO2 and X2O3 in its framework structure, wherein the first zeolitic material has at least one framework structure selected from the group consisting of FAU-, GIS-, MOR-, and LTA-type framework structures; and
(2) heating the mixture obtained in (1) for obtaining a second zeolitic material comprising YO2 and X2O3 in its framework structure, wherein the second zeolitic material obtained in (2) has a different type of framework structure than the first zeolitic material;
wherein the mixture prepared in (1) and heated in (2) contains 1 to 170 wt. % H2O based on 100 wt.-% of YO2 in the framework structure of the first zeolitic material.

### Claim 2 (depends on 1)

The process of claim 1, wherein the second zeolitic material obtained in (2) has a CHA-type framework structure.

### Claim 3 (depends on 1)

The process of claim 1, wherein the one or more structure directing agents comprises one or more tetraalkylammonium cation R1R2R3R4N+-containing compounds, wherein R1, R2, and R3 independently from one another stand for alkyl, and wherein R4 stands for cycloalkyl.

### Claim 4 (depends on 1)

The process of claim 1, wherein the one or more structure directing agents comprises one or more tetraalkylammonium cation R1R2R3R4N+-containing compounds, wherein R1, R2, and R3 independently from one another stand for alkyl, and wherein R4 stands for adamantyl and/or benzyl.

### Claim 5 (depends on 1)

The process of claim 1, wherein the one or more structure directing agents comprises one or more tetraalkylammonium cation R1R2R3R4N+-containing compounds, wherein R1, R2, R3 and R4 independently from one another stand for alkyl, and wherein R3 and R4 form a common alkyl chain.

### Claim 6 (depends on 1)

The process of claim 1, wherein Y is selected from the group consisting of Si, Sn, Ti, Zr, Ge, and a mixture thereof.

### Claim 7 (depends on 1)

The process of claim 1, wherein X is selected from the group consisting of Al, B, In, Ga, and a mixture thereof.

### Claim 8 (depends on 1)

The process of claim 1, wherein the heating (2) is conducted at a temperature ranging from 170 to 300° C.

### Claim 9 (depends on 8)

The process of claim 8, wherein the heating (2) is conducted for a period in the range of from 0.1 h to 6 h.

### Claim 10 (depends on 1)

The process of claim 1, further comprising
(3) calcining the second zeolitic material obtained in (2).

### Claim 11 (depends on 10)

The process of claim 10, further comprising
(4) subjecting the zeolitic material obtained in (2) or (3) to an ion-exchange procedure.

### Claim 12 (depends on 11)

The process of claim 11, further comprising
(5) calcining the zeolitic material obtained in (4).

### Claim 13 (depends on 1)

The process of claim 1, wherein the seed crystals comprise a zeolitic material having a CHA-type and/or an AEI-type framework structure.

### Claim 14 (depends on 1)

A zeolitic material, obtained according to the process of claim 1.

### Claim 15 (depends on 14)

A molecular sieve, an adsorbent, a catalyst, and/or a catalyst support, comprising the zeolitic material of claim 14.