Synthesis of a boron-containing zeolite with an MWW framework structure

Patent metadata

Field	Value
Publication number	US-10793443-B2
Application number	US-201816202918-A
Country	US
Kind code	B2
Filing date	Nov 28, 2018
Priority date	Jun 6, 2014
Publication date	Oct 6, 2020
Grant date	Oct 6, 2020

Abstract

The present invention relates to a process for the production of a boron-containing zeolitic material having an MWW framework structure comprising YO 2 and B 2 O 3 , wherein Y stands for a tetravalent element, wherein said process comprises
(a) providing a mixture comprising one or more sources for YO 2 , one or more sources for B 2 O 3 , one or more organotemplates, and seed crystals,
(b) crystallizing the mixture obtained in (a) for obtaining a layered precursor of the boron-containing MWW-type zeolitic material,
(c) calcining the layered precursor obtained in (b) for obtaining the boron-containing zeolitic material having an MWW framework structure,
wherein the one or more organotemplates have the formula (I)

R 1 R 2 R 3 N  (I)

wherein R 1 is (C 5 -C 8 )cycloalkyl, and

wherein R 2 and R 3 are independently from each other H or alkyl, as well as to a synthetic boron-containing zeolite which is obtainable and/or obtained according to the inventive process as well as to its use.

First claim

The invention claimed is:

1. A synthetic boron-containing zeolitic material having an MWW framework structure, comprising YO 2 and B 2 O 3 , where Y is a tetravalent element,
wherein
the boron-containing zeolitic material is obtained from a process comprising
(a) crystallizing a mixture comprising one or more sources for YO 2 , one or more sources for B 2 O 3 , one or more organotemplates represented by formula (I), and one or more seed crystals, thereby obtaining a layered precursor of the boron-containing MWW-type zeolitic material:
R 1 R 2 R 3 N  (I)

where R 1 is a (C 5 -C 8 )cycloalkyl group, and R 2 and R 3 are independently H or an alkyl group, and
(b) calcining the layered precursor, thereby obtaining the boron-containing zeolitic material having an MWW framework structure.

2. The synthetic boron-containing zeolitic material of claim 1 , wherein the one or more seed crystals comprise YO 2 and X 2 O 3 , where X is a trivalent element selected from the group consisting of Al, B, In, Ga, and any combination thereof.

3. The synthetic boron-containing zeolitic material of claim 1 , wherein the tetravalent element Y is selected from the group consisting of Si, Sn, Ti, Zr, Ge, and any combination thereof.

4. The synthetic boron-containing zeolitic material of claim 1 , wherein
the tetravalent element Y is Si, and
the one or more sources for YO 2 are selected from the group consisting of a silica, a silicate, a silicic acid, and any combination thereof.

5. The synthetic boron-containing zeolitic material of claim 1 , wherein the one or more sources for B 2 O 3 are selected from the group consisting of boric acid, boron oxide, a borate, a borate ester, and any combination thereof.

6. The synthetic boron-containing zeolitic material of claim 1 , wherein a molar ratio of the one or more sources of YO 2 to the one or more sources for B 2 O 3 in the mixture ranges from 1:1 to 300:1.

7. The synthetic boron-containing zeolitic material of claim 1 , wherein the one or more organotemplates are selected from the group consisting of a substituted (C 5 -C 8 )cycloalkylamines, an unsubstituted (C 5 -C 8 )cycloalkylamines, and any combination thereof.

8. The synthetic boron-containing zeolitic material of claim 1 , wherein an amount of the one or more seed crystals in the mixture ranges from 0.05 to 80 weight-% based on 100 weight-% of YO 2 in the one or more sources for YO 2 .

9. The synthetic boron-containing zeolitic material of claim 1 , wherein the crystallizing (a) is conducted under solvothermal conditions.

10. The synthetic boron-containing zeolitic material of claim 1 , wherein the process further comprises, after the crystallizing (a) and before the calcining (b)
(i) isolating the layered precursor obtained in (a),
(ii) optionally washing the layered precursor obtained in (i), and
(iii) optionally drying the layered precursor obtained in (i) or (ii).

11. The synthetic boron-containing zeolitic material of claim 1 , wherein the calcining (b) in the process is carried out at a temperature ranging from 300 to 900° C.

12. The synthetic boron-containing zeolitic material of claim 1 , wherein the process further comprises, after the calcining (b)
(iv) deboronating the boron-containing zeolitic material having an MWW framework structure obtained in (b) with a liquid solvent system, thereby obtaining a deboronated zeolitic material having an MWW framework structure.

13. The synthetic boron-containing zeolitic material of claim 1 , wherein the one or more seed crystals comprise a zeolitic material having an MWW framework structure and/or a layered precursor of a zeolitic material having an MWW framework structure.

14. The synthetic boron-containing zeolitic material of claim 1 , which has a lattice parameter for a c-axis measured from X-ray structure analysis ranging from 25.0 to 27.8 Angstrom.

15. A process, comprising
performing ion-exchange and/or separation of a gas or liquid mixture with the synthetic zeolitic material having an MWW framework of claim 1 as a molecular sieve and/or as an adsorbent comprising contacting said mixture with said synthetic zeolitic material having an MWW framework during said performing.

16. A process, comprising
performing at least one operation selected from the group consisting of hydrocarbon conversion, dehydration, epoxidation, epoxide ring opening, etherification, ammoxidation, and diesel oxidation catalysis with the synthetic zeolitic material having an MWW framework structure of claim 1 as a catalyst and/or as a catalyst component comprising contacting composition with said synthetic zeolitic material having an MWW framework during said performing.

17. The synthetic boron-containing zeolitic material of claim 1 , wherein said one or more organotemplates represented by formula (I) are the only organotemplates.

Assignees

• Basf Se

Inventors

• Maurer Stefan
• Parvulescu Andrei-Nicolae
• Mueller Ulrich
• Meng Xiangju
• Xiao Feng-Shou
• Wang Yeqing

Classifications

• C01B39/48 Primary

  using at least one organic template directing agent · CPC title

• B01D15/361

  Ion-exchange · CPC title

• C01B39/12 Primary

  the replacing atoms being {at least} boron atoms · CPC title

• B01J20/18

  Synthetic zeolitic molecular sieves · CPC title

• B01D2255/50

  Zeolites · CPC title