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US4331641A Expired / Lapsed US ⏱️ 0.0 years remaining

Synthetic crystalline metal silicate compositions and preparation thereof

Assignee: Equistar Chemicals LP
•
Filing: 1979-11-07
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Granted: 1982-05-25
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Expires: 1999-11-07
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Abstract

Abstract Crystalline metal silicate compositions are prepared from a silica containing mixture which is substantially free of aluminum ions and which contains a chelating agent by digesting a reaction mixture comprising, a tetraalkylammonium compound, sodium hydroxide, a metal compound, an oxide of silicon, a chelating agent and water, with the reaction mixture containing less than about 100 ppm aluminum. Crystalline borosilicate compositions are of special interest. A method for activating the new crystalline compositions to enhance their usefulness for certain conversion processes is also disclosed.

Inventors

  • 👤 James A. Hinnenkamp
  • 👤 Vernon V. Walatka, Jr.

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 01:58
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/03; B01J29/035; B01J29/86; C; C01; C01B; C01B35/00; C01B35/08; C01B35/10; C01B35/1009

Claims Analysis

Total Claims: 8
Claim 1
Independent Claim 200 words
A method of preparing a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 / n O:W 2 O 3 :5 to 500 SiO 2 :0 to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises preparing a reaction mixture which is substantially free of aluminum ions and which contains tetraalkylammonium compound, sodium hydroxide, an oxide of the desired metal, an oxide of silicon, water and an aluminum chelating agent effective to provide a catalytically active crystalline metal silicate, maintaining the mixture at an elevated temperature until crystals of said metal silicate are formed and separating and recovering said crystals, and in terms of mole ratios falling within the following ranges, the reaction mixture contains: ______________________________________ OH.sup.- /Si O.sub.2 .05-3 R.sub.4 N.sup.+ /(R.sub.4 N.sup.+ + Na.sup.+) 0.1--H.sub.2 O/OH 10-500 SiO.sub.2 /W.sub.2 O.sub.3 5-500 SiO.sub.2 /Chelating agent 1-1000 ______________________________________ wherein R is propyl.
Claim 2
Independent Claim 200 words
A method of preparing a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 / n O:W 2 O 3 :5 to 500 SiO 2 :0 to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises preparing a reaction mixture which is substantially free of aluminum ions and which contains tetraalkylammonium compound, sodium hydroxide, an oxide of the desired metal, an oxide of silicon, water and an aluminum chelating agent effective to provide a catalytically active crystalline metal silicate, maintaining the mixture at an elevated temperature until crystals of said metal silicate are formed and separating and recovering said crystals, and in terms of mole ratios falling within the following ranges, the reaction mixture contains: ______________________________________ OH.sup.- /Si O.sub.2 .05-3 R.sub.4 N.sup.+ /(R.sub.4 N.sup.+ + Na.sup.+) 0.1--H.sub.2 O/OH 10-500 SiO.sub.2 /W.sub.2 O.sub.3 5-500 SiO.sub.2 /Chelating agent 1-1000 ______________________________________ wherein R is propyl.
Claim 3
Dependent Claim 34 words
A method as in claim 1 wherein the metal is boron and the aluminum content is an amount of less than about 100 wppm based on the weight of silica in the reaction mixture.
Claim 4
Dependent Claim 25 words
A method as in claim 2 wherein the chelating agent is selected from the group consisting of ethylene diamine tetraacetic acid, nitrilioriacetic acid and 8-hydroxyquinoline.
Claim 5
Dependent Claim 15 words
A method as in claim 3 wherein the chelating agent is ethylene diamine tetraacetic acid.
Claim 6
Independent Claim 139 words
A method of activating a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 /nO:W 2 O 3 :5 to 500 SiO 2 :O to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises: (1) Heat treating the dried silicate composition at about 200° to 900° C. (2) Treating the heated silicate with a reducing agent for about 1 to 80 hours at about 200° to 900° C.; and (3) Heat treating the reduced silicate following the procedure of step (1).
Claim 7
Independent Claim 139 words
A method of activating a crystalline metal silicate which is substantially free of aluminum having a composition, in terms of mole ratios as follows: 0.8±0.4 M 2 /nO:W 2 O 3 :5 to 500 SiO 2 :O to 100 H 2 O where M is a cation, n is the valence of said cation and W 2 O 3 is a metal oxide, said metal silicate having the X-ray diffraction pattern set forth in Table 1 of the specification, and a nitrogen isotherm adsorption capacity as shown in FIG. 1 which comprises: (1) Heat treating the dried silicate composition at about 200° to 900° C. (2) Treating the heated silicate with a reducing agent for about 1 to 80 hours at about 200° to 900° C.; and (3) Heat treating the reduced silicate following the procedure of step (1).
Claim 8
Dependent Claim 20 words
A method as in claim 5 wherein the silicate heat treated in step (1) is in the hydrogen ion form.

References Cited (Backward Citations)

US3941871A Cited
US4088605A Cited
DE2746790A1 Cited
US4269813A Cited
US4268420A Cited
US4285919A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1985-05-24 1985-11-23 1986-05-25 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1989-05-24 1989-11-23 1990-05-25 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1993-05-24 1993-11-23 1994-05-25 $7700.00 Window Closed / Lapsed

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