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US4657748A Expired / Lapsed US ⏱️ 0.0 years remaining

Crystalline zeolite (ECR-1) and process for preparing it

Assignee: ExxonMobil Technology and Engineering Co
•
Filing: 1985-03-18
•
Granted: 1987-04-14
•
Expires: 2005-03-18
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Abstract

Abstract A synthetic crystalline zeolite is provided characterized by having a composition, in terms of mole ratios of oxides, in the range: 0.1 to 0.02 R2O:0.90 to 0.98 Na2O:Al2O3:5 to 20 SiO2:0 to 8 H2O wherein R represents a bis-(2-hydroxyethyl) dimethylammonium group, and characterized by having atoms arranged in a structure as indicated by a specified x-ray powder diffraction pattern. The zeolite may be prepared by crystallization from an aged reaction mixture of an oxide of sodium, a bis-(2-hydroxyethyl) dimethylammonium salt, water, a source of silica, a source of alumina, and sodium aluminosilicate nucleating seeds in specified relative amounts.

Inventors

  • 👤 David E. W. Vaughan
  • 👤 Karl G. Strohmaier

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 13:03
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/70; C; C01; C01B; C01B39/00; C01B39/02; C01B39/023; Y; Y10; Y10S; Y10S423/00; Y10S423/25; Y10S423/26

Claims Analysis

Total Claims: 20
Claim 1
Independent Claim 88 words
A synthetic crystalline zeolite characterized by having a composition, in terms of mole ratios of oxides, in the range: 0.5 to 0.02R.sub.2 O:0.90 to 0.98Na.sub.2 O:Al.sub.2 O.sub.3 :5 to 20SiO.sub.2 :xH.sub.2 O wherein R is a tetraalkyl ammonium cation of the type (CH 3 ) 2 R 2 1 N, wherein R 1 is ethyl, propyl, butyl, hydroxyethyl or hydroxypropyl, and x represents 0 or an integer from 1 to 8, and characterized by an x-ray powder diffraction pattern is essentially identical to that given in Table 1.
Claim 2
Dependent Claim 88 words
A synthetic crystalline zeolite characterized by having a composition, in terms of mole ratios of oxides, in the range: 0.5 to 0.02R.sub.2 O:0.90 to 0.98Na.sub.2 O:Al.sub.2 O.sub.3 :5 to 20SiO.sub.2 :xH.sub.2 O wherein R is a tetraalkyl ammonium cation of the type (CH 3 ) 2 R 2 1 N, wherein R 1 is ethyl, propyl, butyl, hydroxyethyl or hydroxypropyl, and x represents 0 or an integer from 1 to 8, and characterized by an x-ray powder diffraction pattern is essentially identical to that given in Table 1.
Claim 3
Dependent Claim 27 words
The zeolite of claim 1 wherein R is partially or fully exchanged with an exchangeable cation selected from Group I through Group VIII of the Periodic Table.
Claim 4
Dependent Claim 22 words
The zeolite of claim 1 having a composition in the range: 0.1 to 0.02R.sub.2 O:0.95 to 0.98Na.sub.2 O:Al.sub.2 O.sub.3 :6 to 10SiO.sub.2.
Claim 5
Dependent Claim 10 words
The zeolite of claim 1 wherein R is bis-(2-hydroxyethyl)dimethyl ammonium.
Claim 6
Dependent Claim 10 words
The zeolite of claim 1 wherein R is bis-(2-hydroxypropyl)dimethyl ammonium.
Claim 7
Dependent Claim 188 words
A process for preparing a crystalline zeolite comprising: (a) preparing a reaction mixture comprising an oxide of sodium, a tetraalkyl ammonium salt, water, a source of silica, a source of alumina and sodium aluminosilicate nucleating seeds, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________ R.sub.2 O:Al.sub.2 O.sub.3 0.2 to 1.0 Na.sub.2 O:Al.sub.2 O.sub.3 1.0 to 7 SiO.sub.2 :Al.sub.2 O.sub.3 5 to 20 H.sub.2 O:Al.sub.2 O.sub.3 120 to 300 R.sub.2 O:Na.sub.2 O 0.05 to 0.4 ______________________________________ where R is a tetraalkyl ammonium cation of the type (CH 3 ) 2 R 2 1 wherein R 1 is ethyl, propyl, butyl, hydroxyethyl or hydroxypropyl, and said seeds being present in an amount to yield 1 to 15 mole percent of the total alumina content of the reaction mixture; (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; (c) maintaining the reaction mixture at between about 120° and 200° C. under autogeneous pressure for a sufficient period of time to form crystals of a zeolite having a composition, in terms of mole ratios of oxides, in the range:
Claim 8
Dependent Claim 188 words
A process for preparing a crystalline zeolite comprising: (a) preparing a reaction mixture comprising an oxide of sodium, a tetraalkyl ammonium salt, water, a source of silica, a source of alumina and sodium aluminosilicate nucleating seeds, said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________ R.sub.2 O:Al.sub.2 O.sub.3 0.2 to 1.0 Na.sub.2 O:Al.sub.2 O.sub.3 1.0 to 7 SiO.sub.2 :Al.sub.2 O.sub.3 5 to 20 H.sub.2 O:Al.sub.2 O.sub.3 120 to 300 R.sub.2 O:Na.sub.2 O 0.05 to 0.4 ______________________________________ where R is a tetraalkyl ammonium cation of the type (CH 3 ) 2 R 2 1 wherein R 1 is ethyl, propyl, butyl, hydroxyethyl or hydroxypropyl, and said seeds being present in an amount to yield 1 to 15 mole percent of the total alumina content of the reaction mixture; (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; (c) maintaining the reaction mixture at between about 120° and 200° C. under autogeneous pressure for a sufficient period of time to form crystals of a zeolite having a composition, in terms of mole ratios of oxides, in the range:
Claim 9
Dependent Claim 52 words
5 to 0.02R 2 O:0.90 to 0.98Na 2 O:Al 2 O 3 :5 to 20SiO 2 :xH 2 O where R and x are defined above, and such that the x-ray powder diffraction pattern of said zeolite is essentially identical to that given in Table I, and (d) recovering said zeolite crystals.
Claim 10
Dependent Claim 52 words
5 to 0.02R 2 O:0.90 to 0.98Na 2 O:Al 2 O 3 :5 to 20SiO 2 :xH 2 O where R and x are defined above, and such that the x-ray powder diffraction pattern of said zeolite is essentially identical to that given in Table I, and (d) recovering said zeolite crystals.
Claim 11
Dependent Claim 10 words
The process of claim 6 wherein R is bis-(2-hydroxyethyl)dimethyl ammonium.
Claim 12
Dependent Claim 10 words
The process of claim 6 where R is bis-(2-hydroxypropyl)dimethyl ammonium.
Claim 13
Dependent Claim 26 words
The process of claim 6 further comprising exchanging the R group with an exchangeable cation selected from Group I through Group VIII of the Periodic Table.
Claim 14
Dependent Claim 27 words
The process of claim 6 wherein the crystalline zeolite product has a composition in the range: 0.1 to 0.02R.sub.2 O:0.95 to 0.98Na.sub.2 O:Al.sub.2 O.sub.3 :6 to 10SiO.sub.2.
Claim 15
Dependent Claim 37 words
The process of claim 6 wherein the source of silica is sodium silicate and the sources of alumina are hydrated alumina and an aluminum salt selected from the group consisting of the chloride, sulfate and nitrate salts.
Claim 16
Dependent Claim 17 words
The process of claim 6 wherein the reaction mixture is maintained at between 140° and 180° C.
Claim 17
Dependent Claim 29 words
The process of claim 6 wherein the seeds are present in an amount to yield 1 to 10 mole percent of the total alumina content of the reaction mixture.
Claim 18
Dependent Claim 13 words
The process of claim 6 wherein said seeds comprise the crystalline zeolite product.
Claim 19
Dependent Claim 206 words
A process for preparing a crystalline zeolite comprising: (a) preparing a reaction mixture comprising sodium aluminate, alum, water, sodium, silicate, aluminum sulfate, bis-(2-hydroxyethyl)dimethylammonium halide, and nucleating seeds of the composition: 13.33Na.sub.2 O:Al.sub.2 O.sub.3 :12.5SiO.sub.2 :267H.sub.2 O said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________ R.sub.2 O:Al.sub.2 O.sub.3 0.1 to 1.0 Na.sub.2 O:Al.sub.2 O.sub.3 1 to 7 SiO.sub.2 :Al.sub.2 O.sub.3 5 to 20 H.sub.2 O:Al.sub.2 O.sub.3 120 to 300 ______________________________________ where R represents a bis-(2-hydroxyethyl)dimethylammonium group, and said seeds being present in an amount to yield 2 to 6 mole percent of the total final alumina content of the reaction mixture; (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; (c) maintaining the reaction mixture at between 140° and 200° C. under autogenous pressure for a sufficient period of time to form crystals of a zeolite having a composition, in terms of mole ratios of oxides, in the range: 0.5 to 0.02R.sub.2 O:0.95 to 0.98Na.sub.2 O:Al.sub.2 O.sub.3 :6 to 10SiO.sub.2 where R is defined above, and having atoms arranged such that the x-ray powder diffraction pattern of said zeolite is essentially identical to that given in Table I; and (d) recovering said zeolite crystals.
Claim 20
Dependent Claim 206 words
A process for preparing a crystalline zeolite comprising: (a) preparing a reaction mixture comprising sodium aluminate, alum, water, sodium, silicate, aluminum sulfate, bis-(2-hydroxyethyl)dimethylammonium halide, and nucleating seeds of the composition: 13.33Na.sub.2 O:Al.sub.2 O.sub.3 :12.5SiO.sub.2 :267H.sub.2 O said reaction mixture having a composition, in terms of mole ratios of oxides, within the following ranges: ______________________________________ R.sub.2 O:Al.sub.2 O.sub.3 0.1 to 1.0 Na.sub.2 O:Al.sub.2 O.sub.3 1 to 7 SiO.sub.2 :Al.sub.2 O.sub.3 5 to 20 H.sub.2 O:Al.sub.2 O.sub.3 120 to 300 ______________________________________ where R represents a bis-(2-hydroxyethyl)dimethylammonium group, and said seeds being present in an amount to yield 2 to 6 mole percent of the total final alumina content of the reaction mixture; (b) blending the reaction mixture sufficiently to form a substantially homogeneous mixture; (c) maintaining the reaction mixture at between 140° and 200° C. under autogenous pressure for a sufficient period of time to form crystals of a zeolite having a composition, in terms of mole ratios of oxides, in the range: 0.5 to 0.02R.sub.2 O:0.95 to 0.98Na.sub.2 O:Al.sub.2 O.sub.3 :6 to 10SiO.sub.2 where R is defined above, and having atoms arranged such that the x-ray powder diffraction pattern of said zeolite is essentially identical to that given in Table I; and (d) recovering said zeolite crystals.

References Cited (Backward Citations)

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US3578723A Cited
US3867512A Cited
US3808326A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1990-04-13 1990-10-13 1991-04-14 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1994-04-13 1994-10-13 1995-04-14 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1998-04-13 1998-10-13 1999-04-14 $7700.00 Window Closed / Lapsed

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