Method for the synthesis of zeolite beta with diethylenetriamine
View Patent ↗A method for the preparation of zeolite beta is described, the template used comprising diethylenetriamine. Furthermore, a zeolite beta obtainable thereby and the preferred use thereof are disclosed.
1. A method for the preparation of zeolite beta the comprising reacting a reaction mixture comprising a template and other components in order to form the zeolite beta, wherein the template used comprises diethylenetriamine.
2. The method as claimed in claim 1 , characterized in that the template used comprises diethylenetriamine and tetraethylammonium cations.
3. The method as claimed in claim 1 , characterized in that the template substantially or completely consists of diethylenetriamine and at least one compound containing tetraethylammonium cations.
4. The method as claimed in claim 3 , characterized in that the reaction mixture has a composition, expressed as molar ratios, in the following ranges:
SiO 2 /Al 2 O 3
from 10 to 400
M 2 O/SiO 2
from 0.001 to 0.1
R 2 O/SiO 2
from 0.04 to 0.5
R′/SiO 2
from 0.05 to 1
H 2 O/SiO 2
from 8 to 300
in which R is a tetraethylammonium salt, R′ is diethylenetriamine and M is an alkali metal ion.
5. The method as claimed in claim 4 , characterized in that R′ is a salt with a general empirical formula selected from R′X, R′X 2 and/or R′X 3 .
6. The method as claimed in claim 5 , wherein R′ comprises a halide.
7. The method as claimed in claim 6 , wherein the halide comprises a bromide.
8. The method as claimed in claim 4 , characterized in that R comprises tetraethylammonium bromide and M comprises sodium.
9. The method as claimed in claim 4 , characterized in that M and/or R and/or R′ are exchanged completely or partly for hydrogen and/or metals of groups IIA, IIIA, IVA, IB, IIB, IIIB, IVB, VIB, and/or VIII of the Periodic Table of the Elements.
10. The method as claimed in claim 9 , wherein M and/or R and/or R′ are exchanged with a metal selected from Cu, Ag, Co, Fe, Ni, platinum metals, and mixtures thereof.
11. The method as claimed in claim 10 , wherein M and/or R and/or R′ are exchanged with a metal selected from Pt, Pd, Rh, Ru, and mixtures thereof.
12. The method as claimed in claim 4 , wherein the tetraethylammonium salt comprises a halide and/or hydroxide.
13. The method as claimed in claim 3 , characterized in that the reaction mixture has the following composition, expressed as molar ratios:
SiO 2 /Al 2 O 3
from 20 to 50
M 2 O/SiO 2
from 0.01 to 0.08
R 2 O/SiO 2
from 0.06 to 0.4
R′/SiO 2
from 0.1 to 0.5
H 2 O/SiO 2
from 10 to 50
in which R is a tetraethylammonium salt, R′ is diethylenetriamine and M is an alkali metal ion.
14. The method as claimed in claim 3 , characterized in that the template further comprises diethylene glycol.
15. The method as claimed in claim 1 , characterized in that the reaction mixture is kept at a temperature of from 100 to 180° C. until crystals of zeolite beta have formed, and then the zeolite crystals obtained are separated off.
16. The method as claimed in claim 1 further comprising adding seed crystals of zeolite beta to the reaction mixture to promote the formation of further crystals of zeolite beta.