Method for making molecular sieve SSZ-99
A method for making a new crystalline molecular sieve designated SSZ-99 is disclosed. SSZ-99 is synthesized using a methylethyldiisopropylammonium cation as a structure directing agent.
1. A method for preparing molecular sieve SSZ-99, comprising:
(a) preparing a reaction mixture containing (1) at least one source of at least one oxide of a tetravalent element; (2) one or more sources of one or more oxides selected from the group consisting of oxides of trivalent elements, pentavalent elements, and mixtures thereof; (3) at least one source of an element selected from Groups 1 and 2 of the Periodic Table; (4) hydroxide ions; (5) a methylethyldiisopropylammonium cation; and (6) water; and
(b) subjecting the reaction mixture to crystallization condition sufficient to form crystals of the molecular sieve.
2. The method of claim 1 , wherein the molecular sieve is prepared from a reaction mixture comprising, in terms of mole ratios, the following:
TO 2 /X 2 O b
5 to 50
M/TO 2
0.01 to 1.0
Q/TO 2
0.05 to 0.50
OH/TO 2
0.10 to 1.0
H 2 O/TO 2
10 to 100
wherein:
(1) T is selected from the group consisting of tetravalent elements from Groups 4-14 of the Periodic Table, and mixtures thereof;
(2) X is selected from the group consisting of trivalent and pentavalent elements from Groups 3-13 of the Periodic Table, and mixtures thereof;
(3) b equals the valence state of X;
(4) M is selected from the group consisting of elements from Groups 1 and 2 of the Periodic Table; and
(5) Q is a methylethyldiisopropylammonium cation.
3. The method of claim 2 , wherein T is selected from Si, Ge, and mixtures thereof.
4. The method of claim 2 , wherein X is selected from B, Al, Ga, In, and mixtures thereof.
5. The method of claim 2 , T is Si and X is Al.
6. The method of claim 2 , wherein the molecular sieve is prepared from a reaction comprising, in terms of mole ratios, the following:
TO 2 /X 2 O b
5 to 50
M/TO 2
0.30 to 0.80
Q/TO 2
0.10 to 0.30
OH/TO 2
0.30 to 0.80
H 2 O/TO 2
20 to 50.
7. The method of claim 1 , wherein the molecular sieve has, in its as-synthesized form, an X-ray diffraction pattern substantially as shown in the following Table:
2-Theta
d-Spacing, nm
Relative Intensity
Peak Broadening
P/N
7.54 ± 0.20
1.172
M
B
L
9.71 ± 0.20
0.910
W
VB
L
12.94 ± 0.20
0.684
W
Sh
H
14.97 ± 0.20
0.591
M
Sh
L
15.92 ± 0.20
0.556
S
Sh
H
17.78 ± 0.20
0.499
M
Sh
H
18.40 ± 0.20
0.482
W
Sh
L
19.86 ± 0.20
0.447
M
B
L
21.26 ± 0.20
0.418
S
VB
L
22.51 ± 0.20
0.395
W
B
L
24.40 ± 0.20
0.365
W
Sh
L
26.10 ± 0.20
0.341
VS
Sh
H
27.35 ± 0.20
0.326
W
B
L
28.17 ± 0.20
0.317
W
B
L.
8. The method of claim 1 , wherein the molecular sieve has a composition, as-synthesized and in the anhydrous state, in terms of mole ratios, as follows:
TO 2 /X 2 O b
5 to 50
Q/TO 2
0.02 to 0.10
M/TO 2
0.02 to 0.15
wherein:
(1) T is selected from the group consisting of tetravalent elements from Groups 4-14 of the Periodic Table, and mixtures thereof;
(2) X is selected from the group consisting of trivalent and pentavalent elements from Groups 3-13 of the Periodic Table, and mixtures thereof;
(3) b equals the valence state of X;
(4) Q is a methylethyldiisopropylammonium cation; and
(5) M is selected from the group consisting of elements from Groups 1 and 2 of the Periodic Table.
9. The method of claim 8 , wherein T is selected from Si, Ge, and mixtures thereof.
10. The method of claim 8 , wherein X is selected from B, Al, Ga, In, and mixtures thereof.
11. The method of claim 8 , T is Si and X is Al.