Process for preparing a titanium-containing zeolitic material having an mww framework structure
US-2015368115-A1 · Dec 24, 2015 · US
US9617163B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9617163-B2 |
| Application number | US-201414512008-A |
| Country | US |
| Kind code | B2 |
| Filing date | Oct 10, 2014 |
| Priority date | Oct 10, 2014 |
| Publication date | Apr 11, 2017 |
| Grant date | Apr 11, 2017 |
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A method for preparing EUO framework type molecular sieve is disclosed using an N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication as a structure directing agent. The EUO framework type molecular sieve, in its as-synthesized form, contains in its intracrystalline pores the N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication.
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The invention claimed is: 1. A method for preparing an EUO framework type molecular sieve, comprising: (a) preparing a reaction mixture containing: (1) at least one source of an oxide of at least one 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) an N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication; and (6) water; and (b) subjecting the reaction mixture to crystallization conditions sufficient to form crystals of the EUO framework type 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 10 to 100 M/TO 2 0.05 to 0.50 Q/TO 2 0.05 to 0.50 OH/TO 2 0.10 to 1.0 H 2 O/TO 2 5 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 an N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication. 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, Fe, and mixtures thereof. 5. The method of claim 2 , wherein T is Si and Xis 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 30 to 80 M/TO 2 0.05 to 0.30 Q/TO 2 0.10 to 0.30 OH/TO 2 0.20 to 0.80 H 2 O/TO 2 10 to 50. 7. 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: TO 2 /X 2 O b 10 to 100 Q/TO 2 0.01 to 0.10 M/TO 2 0.01 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 an N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication; and (5) M is selected from the group consisting of elements from Groups 1 and 2 of the Periodic Table. 8. The method of claim 7 , wherein T is selected from Si, Ge, and mixtures thereof. 9. The method of claim 7 , wherein X is selected from B, Al, Ga, In, Fe and mixtures thereof. 10. The method of claim 7 , wherein T is Si and Xis Al. 11. An EUO framework type molecular sieve having a composition, as-synthesized and in its anhydrous state, in terms of mole ratios, as follows: TO 2 /X 2 O b 10 to 100 Q/TO 2 0.01 to 0.10 M/TO 2 0.01 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 an N,N′-dimethyl-1,4-diazabicyclo[2.2.2]octane dication; and (5) M is selected from the group consisting of elements from Groups 1 and 2 of the Periodic Table. 12. The molecular sieve of claim 11 , wherein T is selected from Si, Ge, and mixtures thereof. 13. The molecular sieve of claim 11 , wherein X is selected from B, Al, Ga, In, Fe and mixtures thereof. 14. The molecular sieve of claim 11 , wherein T is Si and X is Al. 15. The molecular sieve of claim 11 , wherein the molecular sieve has a composition, as-synthesized and in its anhydrous state, in terms of mole ratios, as follows: TO 2 /X 2 O b 30 to 80 Q/TO 2 0.01 to 0.10 M/TO 2 0.01 to 0.15.
using at least one organic template directing agent · CPC title
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