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

Patent metadata

Field	Value
Publication number	US-10196276-B2
Application number	US-201515316220-A
Country	US
Kind code	B2
Filing date	Jun 3, 2015
Priority date	Jun 6, 2014
Publication date	Feb 5, 2019
Grant date	Feb 5, 2019

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, 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 process for producing a boron-containing zeolitic material having an MWW framework structure, the process comprising:
(a) crystallizing a mixture comprising one or more sources for YO 2 where Y is a tetravalent element, one or more sources for B 2 O 3 , one or more organotemplates represented by formula (I) as the only organotemplates, and one or more seed crystals to obtain a layered precursor of the boron-containing zeolitic material having an MWW framework structure:
R 1 R 2 R 3 N  formula (I)

where R 1 is a (C 5 -C 8 )cycloalkyl, and R 2 and R 3 are independently from each other H or an alkyl; and
(b) calcining the layered precursor to obtain the boron-containing zeolitic material having an MWW framework structure comprising YO 2 and B 2 O 3 .

2. The process of claim 1 , wherein the one or more seed crystals comprise YO 2 and X 2 O 3 , where X is at least one trivalent element selected from the group consisting of Al, B, In, and Ga.

3. The process of claim 1 , wherein Y is at least one selected from the group consisting of Si, Sn, Ti, Zr, and Ge.

4. The process of claim 1 , wherein
Y is Si, and
the one or more sources for YO 2 are at least one selected from the group consisting of a silica, a silicate, and silicic acid.

5. The process of claim 1 , wherein the one or more sources for B 2 O 3 are at least one selected from the group consisting of boric acid, boron oxide, a borate, and a borate ester.

6. The process of claim 1 , wherein a molar ratio YO 2 :B 2 O 3 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 process of claim 1 , wherein the one or more organotemplates are at least one selected from the group consisting of a substituted (C 5 -C 8 )cycloalkylamine and an unsubstituted (C 5 -C 8 )cycloalkylamine.

8. The process 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 process of claim 1 , wherein the crystallizing (a) is conducted under a solvothermal condition.

10. The process of claim 1 , further comprising: 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 process of claim 1 , wherein the calcining (b) is carried out at a temperature of from 300 to 900° C.

12. The process of claim 1 , further comprising: 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 process 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 process of claim 1 , wherein in the formula (I), both R 2 and R 3 are H.

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

• C01B39/12 Primary

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

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• B01J20/18

  Synthetic zeolitic molecular sieves · CPC title

• B01D15/361

  Ion-exchange · CPC title