US3947482A
Expired / Lapsed
US
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Method for producing open framework zeolites
Assignee: WR Grace and Co Conn
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Filing: 1974-03-20
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Granted: 1976-03-30
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Expires: 1994-03-20
Abstract
Abstract High purity synthetic zeolites having open frameworks, such as offretite, uncontaminated with detectable traces of other zeolites, can be synthesized by the hydrothermal reaction of a silica source, alumina source, sodium hydroxide and/or potassium hydroxide in the presence of a zeolite nucleation slurry synthesized from a mixture of a silica source, alumina source, sodium hydroxide and/or potassium hydroxide and an organic template agent. The preferred organic template agents are the quaternary compounds wherein the central element is one from Group 5A of the Periodic Table and various conjugated aromatic compounds. The zeolite synthesis mixture itself does not contain any organic ion template agent. With this organic template agent not being required, the nucleation slurry is used to promote crystallization of the synthesis mixture to the open framework type of zeolite.
Inventors
- 👤 Edwin W. Albers
- 👤 David E. W. Vaughan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 01:55
CPC Classifications
C; C01; C01B; C01B39/00; C01B39/02; C01B39/14; C01B39/145; C01B39/04; C01B39/30; C01B39/305
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
170 words
A method of synthesizing zeolites having an open framework and requiring organic template ions comprising: forming a first aqueous mixture of a silica source, alumina source and alkali metal hydroxide in a mole ratio of: 2-8 A 2 O: Al 2 O 3 : 2-20 SiO 2 : 120-400 H 2 O, wherein A 2 O is alkali metal oxide; forming a second aqueous mixture of a silica source, alumina source, alkali metal hydroxide and an organic template compound in a mole ratio of 2-8 Z.sub.2 O: Al.sub.2 O.sub.3 : 2-20 SiO.sub.2 : 120-400 H.sub.2 O, wherein Z 2 O is a mixture of alkali metal oxide and organic template ion; aging said second aqeuous mixture for 12 to 300 hours at about 0° C to 120° C; adding a portion of said second aged aqueous mixture to said first aqueous mixture and maintaining the resulting mixture at about 60° C to 150° C for about 5 to 100 hours; and separating said open framework zeolite from the aqueous mixture.
Claim 2
Independent Claim
170 words
A method of synthesizing zeolites having an open framework and requiring organic template ions comprising: forming a first aqueous mixture of a silica source, alumina source and alkali metal hydroxide in a mole ratio of: 2-8 A 2 O: Al 2 O 3 : 2-20 SiO 2 : 120-400 H 2 O, wherein A 2 O is alkali metal oxide; forming a second aqueous mixture of a silica source, alumina source, alkali metal hydroxide and an organic template compound in a mole ratio of 2-8 Z.sub.2 O: Al.sub.2 O.sub.3 : 2-20 SiO.sub.2 : 120-400 H.sub.2 O, wherein Z 2 O is a mixture of alkali metal oxide and organic template ion; aging said second aqeuous mixture for 12 to 300 hours at about 0° C to 120° C; adding a portion of said second aged aqueous mixture to said first aqueous mixture and maintaining the resulting mixture at about 60° C to 150° C for about 5 to 100 hours; and separating said open framework zeolite from the aqueous mixture.
Claim 3
Dependent Claim
23 words
A method as in claim 1 wherein said second aqueous mixture comprises about 1 to 20 percent by weight of said resulting mixture.
Claim 4
Dependent Claim
45 words
A method as in claim 2 wherein said silica source is selected from the group consisting of amorphous silicas, sodium silicate, potassium silicate and mixtures thereof, and said alumina source is selected from the group consisting of alumina, sodium aluminate, potassium aluminate and mixtures thereof.
Claim 5
Dependent Claim
28 words
A method as in claim 3 wherein said silica source is sodium silicate and said alumina source is selected from the group consisting of alumina or aluminum hydroxide.
Claim 6
Dependent Claim
39 words
A method as in claim 2 wherein said first aqueous mixture has a component ratio of: 1.6 Na.sub.2 O: 2.0 K.sub.2 O: Al.sub.2 O.sub.3 : 10.0 SiO.sub.2 : 160 H.sub.2 O and wherein said open framework zeolite is offretite.
Claim 7
Dependent Claim
62 words
A method as in claim 3 wherein said organic template ion is a Group 5A quaternary compound having the formula: (R.sub.4 M).sup.+A.sup.- wherein R is hydrocarbon radical containing 1 to 7 carbon atoms, M is selected from the group consisting of phosphorous and nitrogen and A - is an anion selected from the group consisting of hydroxide, chloride, sulfate, nitrate or phosphate.
Claim 8
Dependent Claim
38 words
A method as in claim 6 wherein said organic molecule R is selected from the molecule group consisting of tetramethylammonium, tetraethylammonium, tetrapropylammonium, tetrabutylammonium, benzyltrimethylammonium, neopentyltrimethylammonium, tetrabutylphosphonium, benzyltrimethylphosphonium, 1-methyl-1,4 diazoniacyclo (2.2.2) octane, 5-azonia-spiro (4.4) nonane and 6-azonia-spiro (4.5) decane.
Claim 9
Dependent Claim
13 words
A method as in claim 6 wherein said organic molecule R is tetramethylammonium.
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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) | 1979-03-30 | 1979-09-29 | 1980-03-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-03-30 | 1983-09-29 | 1984-03-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-03-30 | 1987-09-29 | 1988-03-30 | $7700.00 | Window Closed / Lapsed |