Method for making molecular sieve SSZ-98

Patent metadata

Field	Value
Publication number	US-9416017-B2
Application number	US-201414323473-A
Country	US
Kind code	B2
Filing date	Jul 3, 2014
Priority date	Jul 3, 2014
Publication date	Aug 16, 2016
Grant date	Aug 16, 2016

Abstract

A method is disclosed for making a new crystalline molecular sieve designated SSZ-98. SSZ-98 has the ERI framework type and is synthesized using a N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication as a structure directing agent.

First claim

The invention claimed is:

1. A method for preparing an ERI framework type molecular sieve, comprising:
(a) preparing a reaction mixture containing: (1) at least one source of silicon oxide; (2) at least one source of aluminum oxide; (3) one or more sources of one or more elements selected from Groups 1 and 2 of the Periodic Table; (4) hydroxide ions; (5) a N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication; (6) optionally, 18-crown-6; and (7) water; and
(b) subjecting the reaction mixture to crystallization conditions 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:

SiO 2 /Al 2 O 3
10 to 50

M/SiO 2
0.01 to 1.0

(Q + A)/SiO 2
0.05 to 0.5

OH/SiO 2
0.1 to 1.0

H 2 O/SiO 2
10 to 50

wherein:
(1) M is selected from the group consisting of elements from Groups 1 and 2 of the Periodic Table;
(2) Q is a N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication, and Q>0; and
(3) A is 18-crown-6, and A≧0.

3. The method of claim 2 , wherein the molecular sieve is prepared from a reaction mixture comprising, in terms of mole ratios, the following:

SiO 2 /Al 2 O 3
20 to 40

M/SiO 2
0.1 to 0.6

(Q + A)/SiO 2
0.1 to 0.5

OH/SiO 2
0.2 to 0.7

H 2 O/SiO 2
10 to 25.

4. The method of claim 2 , wherein M is potassium.

5. The method of claim 2 , wherein M is a combination of potassium and strontium.

6. The method of claim 2 , wherein the reaction mixture further comprises seed crystals having a framework type of ERI, KFI, or a combination thereof.

7. The method of claim 6 , wherein the seed crystals are present in an amount such that the mole ratio of seed crystals/SiO 2 in the reaction mixture is from 0.001 to 0.1.

8. The method of claim 1 , wherein the molecular sieve has less than 2.5% OFF framework type character as determined by X-ray diffraction.

9. The method of claim 1 , wherein the molecular sieve has a composition, as-synthesized and in its anhydrous state, in terms of mole ratios, as follows:

SiO 2 /Al 2 O 3
15 to 50

(Q + A)/SiO 2
0.01 to 0.10

M/SiO 2
0.01 to 0.20

wherein:
(1) Q is a N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication, and Q>0;
(2) A is 18-crown-6, and A≧0; and
(3) M is selected from the group consisting of elements from Groups 1 and 2 of the Periodic Table.

10. 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

 7.78 ± 0.20
1.136
VS

 9.74 ± 0.20
0.907
W

11.79 ± 0.20
0.750
W

13.46 ± 0.20
0.657
S

14.10 ± 0.20
0.627
W

15.53 ± 0.20
0.570
M

16.62 ± 0.20
0.533
W

19.51 ± 0.20
0.455
W

20.56 ± 0.20
0.432
VS

21.40 ± 0.20
0.415
M

23.38 ± 0.20
0.380
S

23.76 ± 0.20
0.374
VS

24.88 ± 0.20
0.358
 W.

Assignees

• Xie Dan
• Zones Stacey Ian
• Lew Christopher Michael
• Davis Tracy Margaret
• Chevron Usa Inc

Inventors

• Xie Dan
• Zones Stacey Ian
• Lew Christopher Michael
• Davis Tracy Margaret

Classifications

• C01P2004/03

  obtained by SEM · CPC title

• B01J29/50

  of the erionite or offretite type, e.g. zeolite T, as exemplified by patent document US2950952 · CPC title

• C01B39/305 Primary

  using at least one organic template directing agent · CPC title

• B01J29/56

  Iron group metals or copper · CPC title

• C01P2002/72

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