# US 2018/0022611 A1 · Process for the preparation of a dealuminated zeolitic material having the bea framework structure

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- Number: US 2018/0022611 A1
- Document ID: US20180022611A1
- Status: Published application
- Kind: A1
- Application number: 15/549,905
- Filed: 2016-02-11
- Published: 2018-01-25
- Earliest claimed: 2015-02-12
- Assignees: BASF SE
- Applicants: BASF SE
- Inventors: Mathias Feyen; Stefan Maurer; Ulrich Mueller; Xinhe Bao; Weiping Zhang; Dirk de Vos; Hermann Gies; Feng-Shou Xiao; Yokoi Toshiyuki; Bilge Yilmaz; Ryoichi Otomo
- Web page: https://patentgrep.com/patent/US20180022611A1

## CPC

- C01B 39/026: {After-treatment}
- B01J 29/7007: {Zeolite Beta}
- C01B 39/46: Other types characterised by their X-ray diffraction pattern and their defined composition {(C01B39/023, C01B39/026, C01B39/06 take precedence)}
- C07C 1/20: starting from organic compounds containing only oxygen atoms as heteroatoms
- B01J 35/70: characterised by their crystalline properties, e.g. semi-crystalline (catalysts comprising carbon B01J21/18; molecular sieves B01J29/00)
- B01J 2229/36: Steaming
- B01J 2229/37: Acid treatment
- B01J 2229/40: Special temperature treatment, i.e. other than just for template removal
- B01J 2235/05: Nuclear magnetic resonance [NMR]
- B01J 2235/15: X-ray diffraction
- C01P 2002/86: by NMR- or ESR-data
- C07C 2529/70: of types characterised by their specific structure not provided for in groups C07C2529/08 - C07C2529/65
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention relates to a method for the preparation of a treated zeolitic material having a BEA framework structure comprising the steps of: (i) providing a zeolitic material having a BEA framework structure, wherein the BEA framework structure comprises YO2 and X2O3, wherein Y is a tetravalent element, and X is a trivalent element, and wherein the zeolitic material having a BEA framework structure is obtainable and/or obtained from an organotemplate-free synthetic process; (ii) calcining the zeolitic material provided in step (i) at a temperature of 650° C. or more; and (iii) treating the calcined zeolitic material obtained from step (ii) with an aqueous solution having a pH of 5 or less, as well as to zeolitic materials per se preferably obtainable according to the inventive method and to their use, and to a process for converting oxygenates to olefins employing the inventive zeolitic materials.

## Claims

### Claim 1

A method for the preparation of a treated zeolitic material having a BEA framework structure comprising the steps of:
(i) providing a zeolitic material having a BEA framework structure, wherein the BEA framework structure comprises YO2 and X2O3, wherein Y is a tetravalent element, and X is a trivalent element, and wherein the zeolitic material having a BEA framework structure is obtainable and/or obtained from an organotemplate-free synthetic process;
(ii) calcining the zeolitic material provided in step (i) at a temperature of 650° C. or more; and
(iii) treating the calcined zeolitic material obtained from step (ii) with an aqueous solution having a pH of 5 or less.

### Claim 2 (depends on 1)

The method of claim 1, wherein in step (ii) the zeolitic material provided in step (i) is calcined at a temperature comprised in the range of from 680° C. to 1000° C.

### Claim 3 (depends on 1)

The method of claim 1, wherein calcining in step (ii) is conducted in an atmosphere containing 10 wt.-% or less of water.

### Claim 4 (depends on 1)

The method of claim 1, wherein Y is selected from the group consisting of Si, Sn, Ti, Zr, Ta, Fe, Ge, and combinations of two or more thereof.

### Claim 5 (depends on 1)

The method of claim 1, wherein X is selected from the group consisting of Al, B, In, Ga, and combinations of two or more thereof.

### Claim 6 (depends on 1)

The method of claim 1, wherein the zeolitic material provided in step (i) is non-calcined.

### Claim 7 (depends on 1)

A zeolitic material having a BEA framework structure obtainable and/or obtained according to a method as defined in claim 1.

### Claim 8

A zeolitic material having a BEA framework structure having an X-ray diffraction pattern comprising at least the following reflections:
Intensity (%)
Diffraction angle 2θ/° [Cu K(alpha 1)]
[8-46]
[21.49-21.79]
100
[22.55-22.85]
[7-37]
[25.45-25.75]
[5-30]
[27.10-27.40]
[4-23]
[28.96-29.26]
[4-23]
[29.75-30.05]
[2-14]
[33.64-33.94]
wherein 100% relates to the intensity of the maximum peak in the X-ray diffraction pattern, and wherein the BEA framework structure comprises YO2 and X2O3, wherein Y is a tetravalent element, and X is a trivalent element.

### Claim 9 (depends on 8)

The zeolitic material of claim 8, wherein the 29Si MAS NMR spectrum of the zeolitic material comprises:
one or more peaks (P′1) in the range of from −95 to −104.5 ppm; and
one or more peaks (P′2) in the range of from −105 to −116 ppm;
wherein the ratio of the total integration value of the one or more peaks (P′1) to the one or more peaks (P′2) is comprised in the range of from 19:81 to 35:65.

### Claim 10

A zeolitic material having a BEA framework structure, wherein the BEA framework structure comprises YO2 and X2O3, wherein Y is a tetravalent element, and X is a trivalent element, and wherein the 27Al MAS NMR of the zeolitic material comprises:
a first peak (P1) in the range of from 45 to 65 ppm;
a second peak (P2) in the range of from 11 to 44 ppm; and
a third peak (P3) in the range of from −10 to 10 ppm;
wherein the integration of the first, second, and third peaks in the 27Al MAS NMR of the zeolitic material offers ratios of the integration values P1:P2:P3 comprised in the range of from 1:(0.1-0.8):(0.4-0.9).

### Claim 11 (depends on 10)

The zeolitic material of claim 10, wherein the zeolitic material is obtainable and/or obtained according to the steps of:
(i) providing a zeolitic material having a BEA framework structure, wherein the BEA framework structure comprises YO2 and X2O3, wherein Y is a tetravalent element, and X is a trivalent element, and wherein the zeolitic material having a BEA framework structure is obtainable and/or obtained from an organotemplate-free synthetic process; and
(ii) calcining the zeolitic material provided in step (i) at a temperature of 650° C. or more.

### Claim 12 (depends on 8)

The zeolitic material of claim 8, wherein Y is selected from the group consisting of Si, Sn, Ti, Zr, Ta, Fe, Ge, and combinations of two or more thereof.

### Claim 13 (depends on 8)

The zeolitic material of claim 8, wherein X is selected from the group consisting of Al, B, In, Ga, and combinations of two or more thereof.

### Claim 14 (depends on 7)

A process for converting oxygenates to olefins, comprising:
(1) providing a gas stream comprising one or more oxygenates;
(2) contacting the gas stream with a catalyst comprising a zeolitic material according to claim 7.

### Claim 15

(canceled)