Zeolite synthesis with a fluoride source
Provided are a novel synthesis technique for producing pure phase aluminosilicate zeolite and a catalyst comprising the phase pure zeolite in combination with a metal, and methods of using the same.
1. A method for making an aluminosilicate zeolite having a CHA framework, the method comprising reacting a synthesis gel comprising zeolite Y, a fluoride source, a structure directing agent (SDA), and an optional additional silica source at a temperature of at least 100° C. until crystals of the zeolite having a CHA framework form.
2. The method of claim 1 , wherein the crystals are at least about 90% phase pure.
3. The method of claim 1 , wherein the crystals have a silica-to-alumina mole ratio (SAR) of at least about 20.
4. The method of claim 1 , wherein the SDA comprises a cation comprising trimethyladamantammonium, N,N,N-dimethylethylcyclohexylammonium, pentamethylimidazolium, 1,2-dimethyl-3-(4-methylbenzyl)imidazolium, 1,2,3-trimethylimidazolium, 1,3-bis(1-adamantyl) imidazolium, 2,6-N,N-diethyl-cis 2,6-dimethylpiperidium, or a combination thereof.
5. The method of claim 1 wherein the crystals have a mean crystal size of less than about 5 μm.
6. The method of claim 1 , wherein the zeolite having a CHA framework comprises crystals with have a mean crystal size of less than about 1 μm.
7. The method of claim 1 wherein the zeolite Y is the only silica and aluminum source to form the aluminosilicate zeolite having a CHA framework.
8. The method of claim 1 , wherein the synthesis gel is substantially free of alkaline metal.
9. The method of claim 1 , wherein the synthesis gel has one or more of the following compositional molar ratios:
SiO 2 /Al 2 O 3 of about 12 to about 500;
SDA 2 O/Al 2 O 3 of about 3 to about 125;
H 2 O/Al 2 O 3 of about 30 to about 7500;
OH − /SiO 2 of about 0.4 to about 0.6; and/or
F − /SiO 2 of about 0.4 to about 0.6.
10. The method of claim 1 , wherein the reacting step is performed at a temperature of about 120 to about 180° C. for about 1 to about 15 days.
11. The method of claim 1 , wherein the reaction step is performed under pH less than about 11.