Crystalline aluminosilicate zeolitic composition: UZM-9
AssigneeUop LLC
InventorsJaime G. Moscoso, Gregory J. Lewis, Jana L. Gisselquist, Mark A. Miller, Lisa M. Rohde
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Abstract
Applicants have synthesized a new aluminosilicate zeolite identified as UZM-9. This new zeolite has the LTA topology and has an empirical formula of: Mmn+Rrp+Al1-xExSiyOz where M is an alkali or alkaline earth metal ion, R is at least two organic ions, at least one of which has an organic group with at least two carbon atoms and E can be gallium, iron, boron and mixtures thereof. The Si/Al ratio can range from greater than 3.5 to about 6.0.
Claims14
A microporous crystalline zeolite having a three dimensional framework of at least AlO2 and SiO2 tetrahedral units and an empirical composition on an as synthesized and anhydrous basis expressed by an empirical formula of:
- Mmn+Rrp+Al1−xExSiyOz
- where M is at least one exchangeable cation selected from the group consisting of alkali and alkaline earth metals, “m” is the mole ratio of M to (Al+E) and varies from 0 to about 0.95, R is at least two organic cations selected from the group consisting of quaternary ammonium ions, diquaternary ammonium ions, protonated amines, protonated alkanolamines and quaternized alkanolammonium ions and further where at least one of said organic cations contains at least one organic group having at least two carbon atoms, “r” is the mole ratio of R to (Al+E) and has a value of about 0.5 to about 1.5, “n” is the weighted average valence of M and has a value of about 1 to about 2, “p” is the weighted average valence of R and has a value of about 1 to about 2, E is an element selected from the group consisting of gallium, iron, boron and mixtures thereof, “x” is the mole fraction of E and has a value from 0 to about 0.5, “y” is the mole ratio of Si to (Al+E) and varies from greater than 3.5 to about 6 and “z” is the mole ratio of O to (Al+E) and has a value determined by the equation:
- z=(m·n+r·p+3+4·y)/2
- and is characterized in that it has the x-ray diffraction pattern having at least the d spacings and intensities set forth in Table A:
- TABLE A 2-θ d(Å) I/I0 % 7.30-7.42 11.9-12.1 m-vs 10.3-10.52 8.4-8.58 m-s 12.65-12.86 6.88-6.99 w-s 14.61-14.85 5.96-6.06 w-m 16.37-16.65 5.32-5.41 w-m 20.74-21.03 4.22-4.28 w-m 21.98-22.38 3.97-4.04 m-vs 23.2-23.64 3.76-3.83 w 24.37-24.78 3.59-3.65 vs 26.51-27.00 3.3-3.36 m 27.51-28.04 3.18-3.24 w-m 30.48-30.81 2.9-2.93 m 31.36-31.82 2.81-2.85 w-m 32.17-33.80 2.65-2.78 w 33.80-34.60 2.59-2.65 w 34.6-35.31 2.54-2.59 w-m 36.19-37.12 2.42-2.48 w 36.96-37.77 2.38-2.43 w 44.83-45.79 1.98-2.02 w-m 48.1-48.93 1.86-1.89 w 48.65-49.5 1.84-1.87 w
A process for preparing a microporous crystalline zeolite having a three dimensional framework of at least AlO2 and SiO2 tetrahedral units and an empirical composition on an as synthesized and anhydrous basis expressed by an empirical formula of:
- Mmn+Rrp+Al1−xExSiyOz
- where M is at least one exchangeable cation selected from the group consisting of alkali and alkaline earth metals, “m” is the mole ratio of M to (Al+E) and varies from 0 to about 0.95, R is at least two organic cations selected from the group consisting of quaternary ammonium ions, diquatemary ammonium ions, protonated amines, piotonated alkanolamines and quaternized alkanolammonium ions and further where at least one of said organic cations contains at least one organic group having at least two carbon atoms, “r” is the mole ratio of R to (Al+E) and has a value of about 0.5 to about 1.5, “n” is the weighted average valence of M and has a value of about 1 to about 2, “p” is the weighted average valence of R and has a value of about 1 to about 2, E is an element selected from the group consisting of gallium, iron, boron and mixtures thereof, “x” is the mole fraction of E and has a value from 0 to about 0.5, “y” is the mole ratio of Si to (Al+E) and varies from greater than 3.5 to about 6 and “z” is the mole ratio of O to (Al+E) and has a value determined by the equation:
- z=(m·n+r·p+3+4·y)/2
- and is characterized in that it has the x-ray diffraction pattern having at least the d spacings and intensities set forth in Table A:
- TABLE A 2-θ d(Å) I/I0 % 7.30-7.42 11.9-12.1 m-vs 10.3-10.52 8.4-8.58 m-s 12.65-12.86 6.88-6.99 w-s 14.61-14.85 5.96-6.06 w-m 16.37-16.65 5.32-5.41 w-m 20.74-21.03 4.22-4.28 w-m 21.98-22.38 3.97-4.04 m-vs 23.2-23.64 3.76-3.83 w 24.37-24.78 3.59-3.65 vs 26.51-27.00 3.3-3.36 m 27.51-28.04 3.18-3.24 w-m 30.48-30.81 2.9-2.93 m 31.36-31.82 2.81-2.85 w-m 32.17-33.80 2.65-2.78 w 33.80-34.60 2.59-2.65 w 34.6-35.31 2.54-2.59 w-m 36.19-37.12 2.42-2.48 w 36.96-37.77 2.38-2.43 w 44.83-45.79 1.98-2.02 w-m 48.1-48.93 1.86-1.89 w 48.65-49.5 1.84-1.87 w
- the process comprising forming a reaction mixture containing reactive sources of M, R, Al, Si and optionally E and reacting the reaction mixture at a temperature of about 60° C. to about 175° C., under autogenous pressure and for a time sufficient to crystallize the microporous crystalline zeolite, the reaction mixture having a composition expressed in terms of mole ratios of the oxides of:
- aM2/nO:bR2/nO:1-cAl2O3:cE2O3:dSiO2:eH2O
- where “a” has a value of 0 to about 1.5, “b” has a value of about 1.0 to about 25, “c” has a value of 0 to about 0.5, “d” has a value of about 6 4 to about 50 and “e” has a value of about 25 to about 15000.
Dependencies are inferred from the claim text.