Molecular sieve SSZ-113 with high acidity, its synthesis and use
View Patent ↗A novel synthetic crystalline molecular sieve material, designated SSZ-113 is provided which exhibits increased acidity. The SSZ-113 can be synthesized using 1,3-bis(2,3-dimethyl-1H-imidazolium)propane dications as a structure directing agent. The synthesis employs a boron pathway to achieve increased acid sites. The SSZ-113 of increased acidity may be used in organic compound conversion and/or sorptive processes.
1 . A method of synthesizing a molecular sieve having an X-ray diffraction pattern including the peaks listed in the following table:
2-Theta
d-Spacing, nm
Relative Intensity
7.80 ± 0.30
1.133
W
9.02 ± 0.30
0.979
VS
9.78 ± 0.30
0.904
M
15.69 ± 0.30
0.564
S
16.72 ± 0.30
0.530
W
18.28 ± 0.30
0.485
VS
21.04 ± 0.30
0.422
W
23.53 ± 0.30
0.378
M
26.22 ± 0.30
0.340
VS
27.36 ± 0.30
0.326
W
and with the molecular sieve comprising boron and having increased acid sites, the method comprising:
(a) providing a reaction mixture comprising:
(1) a source of germanium oxide;
(2) a source of silicon oxide;
(3) a source of boron;
(4) a source of 1,3-bis(2,3-dimethyl-1H-imidazolium)propane dications (Q);
(5) a source of fluoride ions; and
(6) water;
(b) subjecting the reaction mixture to crystallization conditions sufficient to form crystals of the molecular sieve which contains boron;
(c) removing at least some Q; and
(d) replacing some of the boron in the molecular sieve crystals from (c) with aluminum.
2 . The method of claim 1 , wherein the reaction mixture has a composition, in terms of molar ratios, as follows:
(SiO 2 + GeO 2 )/B 2 O 3
≥10
Q/(SiO 2 + GeO 2 )
0.05 to 0.50
F/(SiO 2 + GeO 2 )
0.10 to 1.00
H 2 O/(SiO 2 + GeO 2 + B 2 O 3 )
3 to 8.
3 . The method of claim 1 , wherein the reaction mixture has a composition, in terms of molar ratios, as follows:
(SiO 2 + GeO 2 )/B 2 O 3
15 to 20
Q/(SiO 2 + GeO 2 )
0.05 to 0.50
F/(SiO 2 + GeO 2 )
0.15 to 0.50
H 2 O/(SiO 2 + GeO 2 + B 2 O 3 )
4 to 6.
4 . The method of claim 1 , wherein the source of silicon oxide comprises zeolite Y, having a SiO 2 /Al 2 O 3 ratio of at least 300.
5 . The method of claim 1 , wherein the crystallization conditions include a temperature of from 125° C. to 200° C.
6 . The process of claim 1 , wherein the Q is removed by calcination.
7 . The process of claim 1 , wherein the Q is removed by treatment with ozone.
8 . The process of claim 1 , wherein the replacing of boron with aluminum comprises refluxing the molecular sieve crystals with a solution of aluminum nitrate.