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US4309313A
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Synthesis of cesium-containing zeolite, CSZ-1
Assignee: WR Grace and Co Conn
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Filing: 1980-05-23
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Granted: 1982-01-05
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Expires: 2000-05-23
Abstract
Abstract A new zeolite structure, CSZ-1, has a composition 0.05 to 0.55 M 2 O:0.45 to 0.95 Na 2 O:Al 2 O 3 : 3 to 7 SiO 2 :x H 2 O where M is cesium and/or thallium and x is 0 to 10. The zeolite has utility in sorption, separation and catalytic applications. It is made by reacting together sources of silica, alumina, soda, cesia and/or thallia, together with a nucleating agent or solution, followed by hot aging at a temperature between 50° and 160° C.
Inventors
- 👤 Michael G. Barrett
- 👤 David E. W. Vaughan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 19:27
CPC Classifications
B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/70; B01J29/7019; B01J20/00; B01J20/02; B01J20/10; B01J20/16; B01J20/18; B01J29/80; C; C01; C01B; C01B39/00; C01B39/02; C01B39/20; C01B39/205; C07; C07C; C07C2/00; B01J2229/00; B01J2229/10; B01J2229/26; B01J2229/30; B01J2229/36; B01J2229/42; B01J29/08; B01J29/084; B01J29/085; B01J29/088; C07C2529/00; C07C2529/04; C07C2529/06; C07C2529/70
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
59 words
A synthetic crystalline aluminosilicate zeolite having a formula in terms of mole ratios of oxides as follows: 0.05-0.55 M.sub.2 O:0.45 to 0.95 Na.sub.2 O:Al.sub.2 O.sub.3 :3-7 SiO.sub.2 :x H.sub.2 O where M is cesium or thallium and x is 0 to 10 and having an x-ray powder diffraction pattern substantially as set forth in Table I of the specification.
Claim 2
Dependent Claim
59 words
A synthetic crystalline aluminosilicate zeolite having a formula in terms of mole ratios of oxides as follows: 0.05-0.55 M.sub.2 O:0.45 to 0.95 Na.sub.2 O:Al.sub.2 O.sub.3 :3-7 SiO.sub.2 :x H.sub.2 O where M is cesium or thallium and x is 0 to 10 and having an x-ray powder diffraction pattern substantially as set forth in Table I of the specification.
Claim 3
Dependent Claim
24 words
A composite catalyst consisting of a mixture of the synthetic crystalline aluminosilicate zeolite according to claim 1 and a rare earth exchanged Y zeolite.
Claim 4
Dependent Claim
150 words
A method for preparing the crystalline aluminosilicate zeolite defined in claim 1 which comprises (a) preparing a mixture containing sources of cesia and/or thallia, an oxide of sodium, an oxide of silicon, an oxide of aluminum, water and sodium aluminosilicate nucleating seeds, said mixture having a final composition in terms of mole ratios of oxides and metal atoms within the following ranges M/(M+Na): 0.02-0.3 Na 2 O/SiO 2 : 0.15-0.60 SiO 2 /Al 2 O 3 : 6-30 H 2 O/SiO 2 : 8-50 where M is Cs or T1 and said seeds being present in an amount to yield 0.1 to 25 mole percent of the total final alumina content, (b) mixing the composition of step (a) to obtain a homogeneous reaction mixture which forms a gel, and (c) heating the resulting gel at a temperature of at least 50° C. until the crystals of said zeolite are formed.
Claim 5
Dependent Claim
21 words
The method according to claim 3, wherein the temperature in the heating step is maintained between 50° C. and 160° C.
Claim 6
Dependent Claim
44 words
The method according to claim 3, wherein the amount of reactants is controlled to obtain a final composition n the following ranges Cs/(Cs+Na): 0.02-0.15 Na 2 O/SiO 2 : 0.15-0.60 SiO 2 /Al 2 O 3 : 6-20 H 2 O/SiO 2 : 15-30
Claim 7
Dependent Claim
33 words
The method according to claim 3, wherein the seeds have a composition in terms of mole ratios of oxides of about 16Na 2 O:1-9Al 1 O 3 : 15SiO 2 :250-2000H 2 O.
Claim 8
Dependent Claim
19 words
The method according to claim 3, wherein the nucleating seeds provide the cesia or thallia added in step (a).
Claim 9
Dependent Claim
19 words
The method according to claim 4, wherein the source of cesium is obtained by acid of the mineral pollucite.
Claim 10
Dependent Claim
27 words
The method according to claim 3, wherein the seeds are present in an amount to yield 0.5 to 8 mole percent of the total final alumina content.
Claim 11
Dependent Claim
18 words
The method according to claim 3, further comprising adding alum to neutralize excess caustic obtained from the seeds.
Claim 12
Dependent Claim
22 words
A hydrocarbon conversion catalyst made by substantially exchanging the product of claim 1 with elements of Groups 2-8 of the Periodic Table.
Claim 13
Dependent Claim
24 words
Sorbent compositions comprising the product produced by exchanging the product of claim 1 with cations of elements of Groups 1-8 of the Periodic Table.
Claim 14
Dependent Claim
32 words
A synthetic crystalline aluminosilicate zeolite comprising the product produced by ion exchanging the zeolite of claim 1 with an ammonium solution followed by heating so as to increase the hydrogen ion content.
Claim 15
Dependent Claim
28 words
The method according to claim 3, wherein at least part of the oxide of silicon and at least part of the oxide of aluminium is provided by metakaolin.
Claim 16
Dependent Claim
33 words
The method of making a composite catalyst which comprises conducting the method of claim 3 to make the crystalline aluminosilicate zeolite and adding a rare-earth exchanged Y zeolite to form the composite catalyst.
Claim 17
Dependent Claim
43 words
The method of making a high hydrogen ion content zeolite which comprises conducting the method of claim 3 to produce the zeolite and further exchanging the zeolite obtained with an ammonium solution and heating to increase the hydrogen ion content of the zeolite.
Claim 18
Dependent Claim
28 words
A composite catalyst comprising (a) the catalyst of claim 11 combined with (b) a faujasite zeolite exchanged with cations of elements of Groups 2-8 of the Periodic Table.
Claim 19
Dependent Claim
25 words
The composite catalyst of claim 17, wherein the catalyst of part (a) is rare-earth exchanged and the part (b) faujasite is rare-earth exchanged and calcined.
Claim 20
Dependent Claim
42 words
The composite catalyst of claim 18, further comprising a binder matrix and wherein the rare-earth exchanged part (a) catalyst is present in about 22% by weight and the rare-earth exchanged and calcined part (b) faujasite is present in about 3% by weight.
Claim 21
Dependent Claim
31 words
A composite catalyst comprising: (a) the hydrogen ion exchanged zeolite of claim 13, combined with (b) a faujasite zeolite exchanged with cations of elements of Groups 2-8 of the Periodic Table.
Claim 22
Dependent Claim
16 words
The composite catalyst of claim 20, wherein the part (b) faujasite is rare-earth exchanged and calcined.
Claim 23
Dependent Claim
44 words
The composite catalyst of claim 21, further comprising a binder matrix and wherein the hydrogen ion exchanged zeolite of part (a) is present in about 22% by weight and the rare-earth exchanged and calcined part (b) faujasite is present in about 3% by weight.
Claim 24
Dependent Claim
44 words
The composite catalyst of claim 21, further comprising a binder matrix and wherein the hydrogen ion exchanged zeolite of part (a) is present in about 10% by weight and the rare-earth exchanged and calcined part (b) faujasite is present in about 5% by weight.
Claim 25
Dependent Claim
21 words
A composite catalyst comprising (a) the hydrogen ion exchanged zeolite of claim 13 combined with (b) a hydrogen ion exchanged Y-zeolite.
Claim 26
Dependent Claim
44 words
The composite catalyst of claim 24, further comprising a binder matrix and wherein the hydrogen ion exchanged zeolite of part (a) is present in about 10% by weight and the ydrogen ion exchanged Y-zeolite of part (b) is present in about 10% by weight.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-01-04 | 1985-07-06 | 1986-01-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-01-04 | 1989-07-06 | 1990-01-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-01-04 | 1993-07-06 | 1994-01-05 | $7700.00 | Window Closed / Lapsed |